#------------------------------------------------------------------------------
#$Date: 2025-07-01 13:55:54 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1150 $
#$URL: svn://crystallography.net/testcod/cif/7/20/00/7200031.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7200031
loop_
_publ_author_name
'Marshall, William G.'
'Jones, Richard H.'
'Knight, Kevin S.'
'Clews, John'
'Darton, Richard J.'
'Miller, William'
'Coles, Simon J.'
'Pitak, Mateusz B.'
_publ_section_title
;
 Structural organization in the trimethylamine iodine monochloride complex
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              5194
_journal_page_last               5201
_journal_paper_doi               10.1039/C7CE00869D
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C3 H9 Cl1 I1 N1'
_chemical_formula_sum            'C3 H9 Cl I N'
_chemical_formula_weight         221.47
_chemical_name_common            TMA_ICL
_chemical_name_systematic        'Trimethylamine Iodine Monochloride Complex'
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     Other
_audit_update_record
;
2017-02-08 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.6168(4)
_cell_length_b                   11.1573(3)
_cell_length_c                   10.8342(4)
_cell_measurement_reflns_used    12025
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1404.24(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1607
_diffrn_reflns_theta_full        27.489
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         3.153
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.824
_exptl_absorpt_correction_T_max  0.42
_exptl_absorpt_correction_T_min  0.35
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.81
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9793
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1601
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.0004949
_refine_ls_shift/su_mean         0.0000236
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 12.5 15.8 4.89 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0399
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0399
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1333
_reflns_number_total             1607
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   2.80
_oxford_diffrn_Wilson_scale      10.04
_oxford_refine_ls_r_factor_ref   0.0333
_oxford_refine_ls_scale          0.31166(17)
_oxford_reflns_number_all        1601
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7ce00869d1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C3 H9 Cl1 I1 N1'
_cod_database_code               7200031
_iucr_refine_instruction_details_constraints
;
#
# Punched on 08/12/13 at 01:36:12
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT I    (    1 ,X'S,U'S)  UNTIL C    (    3 ) 
CONT H    (   11 ,X'S,U[ISO])  UNTIL H    (   33 ) 
EQUIV H(11,U[ISO]) UNTIL H(13) 
EQUIV H(21,U[ISO]) UNTIL H(23) 
EQUIV H(31,U[ISO]) UNTIL H(33) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 08/12/13 at 01:36:12
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM NO H   NO #H U MULT DIST 
REM C-H 
REM >4           1.5    .96 DISORDER 
REM 1      1     1.2    .93 C C-H (ACETYLENE) 
REM 1      2     1.2    .93 C-C(H)-C 
REM 1      3     1.2    .98 (C)3-C-H 
REM 2      1     1.2    .93 C=C-H(2) 
REM 2      2     1.2    .97 (C)2-C-(H)2 
REM 3      1     1.5    .96 C-C-(H)3 
REM N-H 
REM >4           1.5    .89 DISORDER 
REM 1      1     1.2    .86 N-N/H 
REM 1      2     1.2    .86 (C)2-N-H 
REM 1      3     1.2    .89 (C)3-N-H 
REM 2      1     1.2    .86 C-N-(H)2 
REM 2      2     1.2    .89 (C)2-N-(H)2 
REM 3      1     1.2    .89 C-H-(H)3 
REM O-H 
REM 1      1     1.5    .82 O-H 
REM 
REM DIST      ESD = 0.02 
REM VIB       ESD = 0.002 
REM ANGLE     ESD = 2.0 
REM            3 H ON SP 3 
ANGLE 109.54, 3.0 = 
CONT N(3) TO C ( 1) TO H(11) 
CONT N(3) TO C ( 1) TO H(12) 
CONT N(3) TO C ( 1) TO H(13) 
ANGLE 0.0, 3.0 = MEAN H(11) TO C ( 1) TO H(12) 
CONT H(11) TO C ( 1) TO H(13) 
CONT H(12) TO C ( 1) TO H(13) 
REM            3 H ON SP 3 
ANGLE 109.54, 3.0 = 
CONT N(3) TO C ( 2) TO H(21) 
CONT N(3) TO C ( 2) TO H(22) 
CONT N(3) TO C ( 2) TO H(23) 
ANGLE 0.0, 3.0 = MEAN H(21) TO C ( 2) TO H(22) 
CONT H(21) TO C ( 2) TO H(23) 
CONT H(22) TO C ( 2) TO H(23) 
REM            3 H ON SP 3 
ANGLE 109.54, 3.0 = 
CONT N(3) TO C ( 3) TO H(31) 
CONT N(3) TO C ( 3) TO H(32) 
CONT N(3) TO C ( 3) TO H(33) 
ANGLE 0.0, 3.0 = MEAN H(31) TO C ( 3) TO H(32) 
CONT H(31) TO C ( 3) TO H(33) 
CONT H(32) TO C ( 3) TO H(33) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
x+1/2,-y+1/2,-z
-x+1/2,y+1/2,z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
I1 I 0.40237(2) 0.36577(2) 0.60062(2) 0.0329 1.0000 Uani . . . . . .
Cl2 Cl 0.52611(10) 0.25519(12) 0.44140(11) 0.0527 1.0000 Uani . . . . . .
N3 N 0.2936(3) 0.4629(3) 0.7477(3) 0.0342 1.0000 Uani D . . . . .
C1 C 0.2333(4) 0.3715(5) 0.8233(4) 0.0470 1.0000 Uani D . . . . .
C2 C 0.3709(4) 0.5357(4) 0.8256(5) 0.0461 1.0000 Uani D . . . . .
C3 C 0.2082(4) 0.5404(5) 0.6854(5) 0.0549 1.0000 Uani D . . . . .
H11 H 0.185(4) 0.410(3) 0.894(5) 0.063(9) 1.0000 Uiso D . . . . .
H12 H 0.180(4) 0.320(3) 0.768(4) 0.064(9) 1.0000 Uiso D . . . . .
H13 H 0.294(4) 0.322(4) 0.865(4) 0.064(9) 1.0000 Uiso D . . . . .
H21 H 0.325(3) 0.580(4) 0.886(4) 0.065(9) 1.0000 Uiso D . . . . .
H22 H 0.425(4) 0.483(4) 0.868(4) 0.065(9) 1.0000 Uiso D . . . . .
H23 H 0.417(4) 0.597(4) 0.770(4) 0.065(9) 1.0000 Uiso D . . . . .
H31 H 0.157(4) 0.577(3) 0.751(4) 0.067(9) 1.0000 Uiso D . . . . .
H32 H 0.248(3) 0.605(4) 0.637(4) 0.067(9) 1.0000 Uiso D . . . . .
H33 H 0.166(3) 0.497(4) 0.632(4) 0.067(9) 1.0000 Uiso D . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.03185(12) 0.03428(12) 0.03266(12) 0.00051(11) 0.00045(11) -0.00169(11)
Cl2 0.0548(6) 0.0538(6) 0.0495(6) -0.0140(5) 0.0111(6) -0.0002(6)
N3 0.0312(16) 0.0346(17) 0.0368(17) 0.0025(16) 0.0030(15) 0.0018(15)
C1 0.041(2) 0.048(3) 0.053(3) 0.003(2) 0.014(2) -0.012(2)
C2 0.046(3) 0.046(3) 0.046(3) -0.009(2) 0.002(2) -0.006(2)
C3 0.050(3) 0.060(3) 0.055(3) 0.001(3) -0.004(2) 0.024(3)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776
4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl2 . I1 . N3 . 178.58(9) yes
I1 . N3 . C1 . 108.5(3) yes
I1 . N3 . C2 . 108.7(3) yes
C1 . N3 . C2 . 110.5(3) yes
I1 . N3 . C3 . 109.1(3) yes
C1 . N3 . C3 . 109.7(4) yes
C2 . N3 . C3 . 110.3(3) yes
N3 . C1 . H11 . 111.8(19) no
N3 . C1 . H12 . 110.0(19) no
H11 . C1 . H12 . 109(2) no
N3 . C1 . H13 . 107.5(19) no
H11 . C1 . H13 . 106(2) no
H12 . C1 . H13 . 112(2) no
N3 . C2 . H21 . 109.2(20) no
N3 . C2 . H22 . 109.6(19) no
H21 . C2 . H22 . 110(2) no
N3 . C2 . H23 . 110.1(18) no
H21 . C2 . H23 . 109(2) no
H22 . C2 . H23 . 109(2) no
N3 . C3 . H31 . 108.2(20) no
N3 . C3 . H32 . 111(2) no
H31 . C3 . H32 . 110(2) no
N3 . C3 . H33 . 110(2) no
H31 . C3 . H33 . 110(2) no
H32 . C3 . H33 . 108(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I1 . Cl2 . 2.5621(12) yes
I1 . N3 . 2.304(3) yes
N3 . C1 . 1.485(5) yes
N3 . C2 . 1.476(5) yes
N3 . C3 . 1.478(5) yes
C1 . H11 . 1.04(5) no
C1 . H12 . 1.03(5) no
C1 . H13 . 1.00(5) no
C2 . H21 . 0.97(5) no
C2 . H22 . 0.98(5) no
C2 . H23 . 1.06(5) no
C3 . H31 . 1.01(5) no
C3 . H32 . 1.01(5) no
C3 . H33 . 0.90(5) no
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 2 3 x .
