The crystal structure of dichlorido-(tris(2-benzimidazolylmethyl)amine-κ4 N,N′,N′′,N′′′)chromium(III) chloride — methanol (1/3), CrC27H33Cl3N7O3
Li, Ji; Wu, Siqi; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 285–287; doi:10.1515/ncrs-2019-0607

data_8105084
_publ_section_title
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 The crystal structure of
 dichlorido-(tris(2-benzimidazolylmethyl)amine-\k4
 N,N&#x2032;,N&#x2032;&#x2032;,N&#x2032;&#x2032;&#x2032;)chromium(III)
 chloride --- methanol (1/3), CrC27H33Cl3N7O3
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_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              285
_journal_page_last               287
_journal_paper_doi               10.1515/ncrs-2019-0607
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C24 H21 Cl2 Cr N7, 3(C H4 O), Cl'
_chemical_formula_sum            'C27 H33 Cl3 Cr N7 O3'
_chemical_formula_weight         661.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                84.163(2)
_cell_angle_beta                 73.602(3)
_cell_angle_gamma                85.524(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7862(13)
_cell_length_b                   12.4690(17)
_cell_length_c                   12.8413(17)
_cell_measurement_reflns_used    5886
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.67
_cell_measurement_theta_min      2.24
_cell_volume                     1493.4(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2003) [2]'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2003)'
_computing_molecular_graphics    'Diamond (Brandenburg, 2006)[5]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[6]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015) [3-4]'
_computing_structure_solution    'ShelXS (Sheldrick, 2015) [3-4]'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13443
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.250
_diffrn_reflns_theta_min         1.644
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick, 2008) [7]'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7221
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+0.6546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1524
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5873
_reflns_number_total             7221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0607_suppl.cif
_cod_data_source_block           i
_cod_database_code               8105084
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.903
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1 = O2-H2
 0.84 with sigma of 0.01
 N3-H3 = N5-H5A = N7-H7A
 0.88 with sigma of 0.01
 C27-O3 \\sim C27-O3'
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O3')
4. Others
 Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(O3')=Sof(H3')=1-FVAR(1)
 Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(O3)=Sof(H3A)=FVAR(1)
5.a Riding coordinates:
 C27(H27A,H27B,H27C,H27D,H27E,H27F), O3(H3A), O3'(H3')
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C9(H9A,H9B), C17(H17A,H17B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15),
 C20(H20), C21(H21), C22(H22), C23(H23)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
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