Dimetalla-heterocyclic carbenes: the interconversion of chalcocarbonyl and carbido ligands.
Barnett, Harrison J.; Hill, Anthony F.; Chemical communications (Cambridge, England) 56 (2020) 12593–12596; doi:10.1039/d0cc05106c

data_7127191
_publ_section_title
;
 Dimetalla-heterocyclic carbenes: the interconversion of chalcocarbonyl
 and carbido ligands.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12593
_journal_page_last               12596
_journal_paper_doi               10.1039/d0cc05106c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C57 H52 Cl2 O5 P4 Rh2 S, C H Cl3'
_chemical_formula_sum            'C58 H53 Cl5 O5 P4 Rh2 S'
_chemical_formula_weight         1369.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-20 deposited with the CCDC.	2020-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.4550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7306(2)
_cell_length_b                   15.6417(3)
_cell_length_c                   30.6406(4)
_cell_measurement_reflns_used    7029
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      70.8700
_cell_measurement_theta_min      4.6230
_cell_volume                     6095.81(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.964
_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    -82.00  -6.00   1.00   15.00    --  -36.03 125.00 120.00   76
  2  \w    -47.00  27.00   1.00   15.00    --  -36.03  57.00   0.00   74
  3  \w     27.00  84.00   1.00   15.00    --   36.03-125.00  90.00   57
  4  \w     27.00  84.00   1.00   15.00    --   36.03-125.00 -60.00   57
  5  \w     36.00 106.00   1.00   70.00    --  105.15 -95.00 150.00   70
  6  \w     49.00 123.00   1.00   70.00    --  105.15 -61.00 -60.00   74
  7  \w    114.00 169.00   1.00   70.00    --  105.15  77.00 -30.00   55
  8  \w     36.00  85.00   1.00   70.00    --  105.15 -95.00-120.00   49
  9  \w     56.00 121.00   1.00   70.00    --  105.15 -45.00-150.00   65
 10  \w     88.00 121.00   1.00   70.00    --  105.15  45.00   0.00   33
 11  \w     92.00 160.00   1.00   70.00    --  105.15  61.00  60.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1161063000
_diffrn_orient_matrix_UB_12      0.0281121000
_diffrn_orient_matrix_UB_13      -0.0040106000
_diffrn_orient_matrix_UB_21      0.0192014000
_diffrn_orient_matrix_UB_22      0.0625172000
_diffrn_orient_matrix_UB_23      0.0383297000
_diffrn_orient_matrix_UB_31      0.0290984000
_diffrn_orient_matrix_UB_32      0.0707104000
_diffrn_orient_matrix_UB_33      -0.0323030000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            19450
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.045
_diffrn_reflns_theta_min         4.041
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.075
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       plate
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.032
_refine_diff_density_max         1.190
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         11380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0609P)^2^+11.7057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1282
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9442
_reflns_number_total             11380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05106c2.cif
_cod_data_source_block           hb_1234-1-1_scale
_cod_depositor_comments
'Adding full bibliography for 7127189--7127192.cif.'
_cod_database_code               7127191
_publcif_datablock.id            {5e4cbb30-8cc3-4d18-877a-ae5159864aef}
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Ternary CH refined with riding coordinates:
 C101(H101)
2.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B)
2.d Aromatic/amide H refined with riding coordinates:
 C85(H85), C35(H35), C44(H44), C64(H64), C55(H55), C15(H15), C66(H66),
 C13(H13), C26(H26), C84(H84), C32(H32), C25(H25), C34(H34), C56(H56), C45(H45),
  C63(H63), C16(H16), C86(H86), C72(H72), C53(H53), C22(H22), C54(H54),
 C82(H82), C46(H46), C23(H23), C74(H74), C14(H14), C76(H76), C73(H73), C12(H12),
  C62(H62), C52(H52), C42(H42), C36(H36), C33(H33), C65(H65), C43(H43),
 C24(H24), C83(H83), C75(H75)
2.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              85959
_shelx_fab_checksum              48971
_ins_header
;
TITL HB_1234-1-1_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  12.730618  15.641651  30.640578  90.0000  92.4550  90.0000
ZERR    4.00   0.000226   0.000277   0.000427   0.0000   0.0014   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H O P S Cl Rh
UNIT 224.00 188.00 20.00 16.00 4.00 20.00 8.00
TREF
HKLF 4
END
;
_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 1.523
_oxdiff_exptl_absorpt_empirical_full_min 0.766
_publcif_funding_html
;
;