#------------------------------------------------------------------------------ #$Date: 2025-07-01 13:55:54 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1150 $ #$URL: svn://localhost/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 '\f & \w 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/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ 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>2.0\s(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 .