Synthesis, structural characterization, and coordination chemistry of imidazole-based alkylidene ketenes.
Feuerstein, Wolfram; Varava, Paul; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Severin, Kay; Chemical communications (Cambridge, England) 57 (2021) 11509–11512; doi:10.1039/d1cc05161j

data_7129122
_publ_section_title
;
 Synthesis, structural characterization, and coordination chemistry of
 imidazole-based alkylidene ketenes.
;
_journal_issue                   87
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11509
_journal_page_last               11512
_journal_paper_doi               10.1039/d1cc05161j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C31 H36 Cl N2 O3 Rh'
_chemical_formula_sum            'C31 H36 Cl N2 O3 Rh'
_chemical_formula_weight         622.98
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-11-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.0954(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.32987(14)
_cell_length_b                   14.7730(2)
_cell_length_c                   20.5303(3)
_cell_measurement_reflns_used    9073
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.4480
_cell_measurement_theta_min      3.6780
_cell_volume                     3093.60(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_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   -109.00 -12.00   1.00    1.00    --  -40.91 -60.00 178.00   97
  2  \w    -11.00  32.00   1.00    1.00    --  -40.91  60.00 -41.00   43
  3  \w    -56.00 -21.00   1.00    1.00    --  -40.91  60.00 -41.00   35
  4  \w     -5.00  20.00   1.00    1.00    --   40.91 -60.00 178.00   25
  5  \w     87.00 175.00   1.00    4.00    --  105.15  60.00 -41.00   88
  6  \w     35.00 130.00   1.00    4.00    --  105.15 -60.00 178.00   95
  7  \w     37.00  85.00   1.00    1.00    --   40.91-125.00 120.00   48
  8  \w     30.00  96.00   1.00    1.00    --   40.91-125.00  30.00   66
  9  \w     17.00  45.00   1.00    1.00    --   40.91 -99.00-180.00   28
 10  \w     38.00  63.00   1.00    1.00    --   40.91  60.00 -41.00   25
 11  \w    103.00 171.00   1.00    4.00    --  105.15  77.00  30.00   68
 12  \w     96.00 146.00   1.00    4.00    --  105.15 178.00  90.00   50
 13  \w    104.00 158.00   1.00    4.00    --  105.15  77.00   0.00   54
 14  \w    103.00 168.00   1.00    4.00    --  105.15  77.00 -90.00   65
 15  \w    113.00 168.00   1.00    4.00    --  105.15 111.00-150.00   55
 16  \w    135.00 174.00   1.00    4.00    --  105.15 111.00-120.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1406012000
_diffrn_orient_matrix_UB_12      -0.0268471000
_diffrn_orient_matrix_UB_13      -0.0081970000
_diffrn_orient_matrix_UB_21      0.0043013000
_diffrn_orient_matrix_UB_22      -0.0683677000
_diffrn_orient_matrix_UB_23      0.0569604000
_diffrn_orient_matrix_UB_31      -0.0549414000
_diffrn_orient_matrix_UB_32      -0.0740562000
_diffrn_orient_matrix_UB_33      -0.0496332000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15548
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.620
_diffrn_reflns_theta_min         3.702
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.509
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         6015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0255P)^2^+2.0812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5408
_reflns_number_total             6015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05161j2.cif
_cod_data_source_block           pv213_c
_cod_depositor_comments
'Adding full bibliography for 7129122--7129133.cif.'
_cod_original_cell_volume        3093.59(7)
_cod_database_code               7129122
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C31 H36 N2 O3 Cl1 Rh1'
_shelx_estimated_absorpt_t_max   0.490
_shelx_estimated_absorpt_t_min   0.422
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_shelx_res_checksum              49490
_shelx_hkl_checksum              95213
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.447
_oxdiff_exptl_absorpt_empirical_full_min 0.824