The crystal structure tetrakis(μ2-o-chlorobenzoato-κ2 O:O′)-bis(methanol-κ1 O)dirhodium(II), C30H24Cl4O10Rh2
Zhu, Guangyuan; Meng, Miao; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 867–868; doi:10.1515/ncrs-2020-0067

data_8105313
_publ_section_title
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 The crystal structure tetrakis(\m2-o-chlorobenzoato-\k2
 O:O&#x2032;)-bis(methanol-\k1 O)dirhodium(II), C30H24Cl4O10Rh2
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_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              867
_journal_page_last               868
_journal_paper_doi               10.1515/ncrs-2020-0067
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C30 H24 Cl4 O10 Rh2'
_chemical_formula_sum            'C30 H24 Cl4 O10 Rh2'
_chemical_formula_weight         892.14
_chemical_name_systematic
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The crystal structure of Rhodium(II) o-Chlorobenzoate Dimer with axial 
Methanol Molecules, C~30~H~24~Cl~4~O~10~Rh~2~
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 91.780(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5270(4)
_cell_length_b                   12.3533(6)
_cell_length_c                   17.4904(8)
_cell_measurement_reflns_used    3564
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.8840
_cell_measurement_theta_min      6.2070
_cell_volume                     1625.53(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9646
_diffrn_measured_fraction_theta_max 0.9646
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     45.00  83.00   0.50    0.50    --    0.00  38.00-120.00   76
  2  \w     -7.00  18.00   0.50    0.50    --    0.00  38.00-120.00   50
  3  \w    -89.00   7.00   0.50    0.50    --    0.00 -38.00   0.00  192
  4  \w     24.00  51.00   0.50    0.50    --    0.00  38.00  30.00   54
  5  \w     86.00 152.00   0.50    1.00    --   95.20  45.00-180.00  132
  6  \w     76.00 169.00   0.50    1.00    --   95.20  45.00 120.00  186
  7  \w      8.00 118.00   0.50    1.00    --   95.20 -61.00 -90.00  220
  8  \w     76.00 182.00   0.50    1.00    --   95.20  45.00 150.00  212
  9  \w     66.00  91.00   0.50    1.00    --   95.20 -30.00 -60.00   50
 10  \w     76.00 184.00   0.50    1.00    --   95.20  82.00  30.00  216
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1089687000
_diffrn_orient_matrix_UB_12      -0.0987705000
_diffrn_orient_matrix_UB_13      -0.0250316000
_diffrn_orient_matrix_UB_21      -0.0411627000
_diffrn_orient_matrix_UB_22      0.0282704000
_diffrn_orient_matrix_UB_23      -0.0844714000
_diffrn_orient_matrix_UB_31      0.1683838000
_diffrn_orient_matrix_UB_32      0.0707435000
_diffrn_orient_matrix_UB_33      -0.0012038000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7741
_diffrn_reflns_theta_full        74.0243
_diffrn_reflns_theta_max         74.02
_diffrn_reflns_theta_min         4.38
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.8226
_exptl_crystal_description       needle
_exptl_crystal_F_000             889.8180
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.1227
_refine_diff_density_min         -1.9141
_refine_diff_density_rms         0.1619
_refine_ls_d_res_high            0.8019
_refine_ls_d_res_low             10.0887
_refine_ls_goodness_of_fit_ref   1.0278
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    21
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3185
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0273
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+3.3428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -9
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -7
_reflns_number_gt                2824
_reflns_number_total             3185
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2020-0067_suppl.cif
_cod_data_source_block           Rh2-2-Cl-2
_cod_original_cell_volume        1625.52(14)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               8105313
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C14-H5
 1.870703 with sigma of 0.02
 Rh1-H5
 2.917619 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C0(H0), C4(H4), C5(H5a), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12)
3.b Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.840
_oxdiff_exptl_absorpt_empirical_full_min 0.616