#------------------------------------------------------------------------------ #$Date: 2025-07-01 13:55:54 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1150 $ #$URL: svn://localhost/testcod/cif/7/20/00/7200032.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_7200032 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 TAMICl _chemical_name_systematic 'Trimethylamine Iodine momochloride comples' _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 11.5039(3) _cell_length_b 10.9570(3) _cell_length_c 10.6758(3) _cell_measurement_reflns_used 10668 _cell_measurement_temperature 110 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.91 _cell_volume 1345.67(6) _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 110 _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 0.030 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 9192 _diffrn_reflns_theta_full 27.464 _diffrn_reflns_theta_max 27.464 _diffrn_reflns_theta_min 3.199 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.034 _exptl_absorpt_correction_T_max 0.40 _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.186 _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 0.56 _refine_diff_density_min -0.79 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0001 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 85 _refine_ls_number_reflns 1539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0207 _refine_ls_shift/su_max 0.0007647 _refine_ls_shift/su_mean 0.0000320 _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: 14.2 18.1 6.17 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0353 _refine_ls_wR_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0353 _reflns_limit_h_max 14 _reflns_limit_h_min 0 _reflns_limit_k_max 14 _reflns_limit_k_min 0 _reflns_limit_l_max 13 _reflns_limit_l_min 0 _reflns_number_gt 1418 _reflns_number_total 1539 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 0.79 _oxford_diffrn_Wilson_scale 12.16 _oxford_refine_ls_r_factor_ref 0.0237 _oxford_refine_ls_scale 0.28878(14) _oxford_reflns_number_all 1539 _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 7200032 _iucr_refine_instruction_details_constraints ; # # Punched on 08/12/13 at 01:42:51 # #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 01:42:51 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) 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 0.404991(16) 0.366499(17) 0.601730(18) 0.0095 1.0000 Uani . . . . . . Cl2 Cl 0.53050(7) 0.25578(8) 0.43695(7) 0.0155 1.0000 Uani . . . . . . N3 N 0.2952(2) 0.4625(2) 0.7523(2) 0.0101 1.0000 Uani . . . . . . C1 C 0.2359(3) 0.3675(3) 0.8278(3) 0.0148 1.0000 Uani . . . . . . C2 C 0.3732(3) 0.5367(3) 0.8318(3) 0.0150 1.0000 Uani . . . . . . C3 C 0.2077(3) 0.5413(3) 0.6899(3) 0.0159 1.0000 Uani . . . . . . H11 H 0.187(3) 0.404(3) 0.900(4) 0.019(6) 1.0000 Uiso . . . . . . H12 H 0.182(3) 0.318(3) 0.768(4) 0.019(6) 1.0000 Uiso . . . . . . H13 H 0.290(3) 0.313(4) 0.863(4) 0.019(6) 1.0000 Uiso . . . . . . H21 H 0.329(4) 0.577(4) 0.894(4) 0.022(6) 1.0000 Uiso . . . . . . H22 H 0.432(3) 0.485(4) 0.872(4) 0.022(6) 1.0000 Uiso . . . . . . H23 H 0.419(3) 0.603(3) 0.778(4) 0.022(6) 1.0000 Uiso . . . . . . H31 H 0.162(4) 0.580(3) 0.756(4) 0.023(6) 1.0000 Uiso . . . . . . H32 H 0.243(4) 0.603(4) 0.646(4) 0.023(6) 1.0000 Uiso . . . . . . H33 H 0.157(4) 0.491(4) 0.638(4) 0.023(6) 1.0000 Uiso . . . . . . 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 0.00949(9) 0.00973(9) 0.00918(8) 0.00016(7) 0.00031(7) -0.00037(8) Cl2 0.0166(3) 0.0157(3) 0.0141(4) -0.0039(3) 0.0032(3) -0.0001(3) N3 0.0094(11) 0.0115(12) 0.0095(12) 0.0006(11) 0.0013(10) 0.0009(10) C1 0.0144(15) 0.0134(14) 0.0165(15) 0.0033(14) 0.0045(13) -0.0008(13) C2 0.0158(16) 0.0157(15) 0.0135(15) -0.0038(13) -0.0022(12) -0.0008(13) C3 0.0170(15) 0.0130(15) 0.0178(16) 0.0011(13) -0.0015(13) 0.0071(13) 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 . 178.65(7) yes I1 . N3 . C1 . 108.15(19) yes I1 . N3 . C2 . 108.61(19) yes C1 . N3 . C2 . 110.7(3) yes I1 . N3 . C3 . 108.98(19) yes C1 . N3 . C3 . 109.9(2) yes C2 . N3 . C3 . 110.5(2) yes N3 . C1 . H11 . 113(2) no N3 . C1 . H12 . 108(2) no H11 . C1 . H12 . 109(3) no N3 . C1 . H13 . 111(2) no H11 . C1 . H13 . 108(3) no H12 . C1 . H13 . 108(3) no N3 . C2 . H21 . 110(2) no N3 . C2 . H22 . 110(2) no H21 . C2 . H22 . 110(3) no N3 . C2 . H23 . 111(2) no H21 . C2 . H23 . 109(3) no H22 . C2 . H23 . 107(3) no N3 . C3 . H31 . 107(2) no N3 . C3 . H32 . 111(3) no H31 . C3 . H32 . 107(3) no N3 . C3 . H33 . 109(2) no H31 . C3 . H33 . 110(3) no H32 . C3 . H33 . 113(3) 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 . 2.5790(8) yes I1 . N3 . 2.299(3) yes N3 . C1 . 1.483(4) yes N3 . C2 . 1.478(4) yes N3 . C3 . 1.484(4) yes C1 . H11 . 1.03(4) no C1 . H12 . 1.04(4) no C1 . H13 . 0.94(4) no C2 . H21 . 0.95(4) no C2 . H22 . 0.98(4) no C2 . H23 . 1.07(4) no C3 . H31 . 0.98(4) no C3 . H32 . 0.92(4) no C3 . H33 . 0.97(4) no