Simple generation of a dirhodium μ-carbido complex via thiocarbonyl reduction.
Barnett, Harrison J.; Burt, Liam K.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9570–9574; doi:10.1039/c8dt02524j

data_7046909
_publ_section_title
;
 Simple generation of a dirhodium \m-carbido complex via thiocarbonyl
 reduction.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9570
_journal_page_last               9574
_journal_paper_doi               10.1039/c8dt02524j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C49 H59 B2 N12 P Rh2'
_chemical_formula_sum            'C49 H59 B2 N12 P Rh2'
_chemical_formula_weight         1074.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-03 deposited with the CCDC.
2018-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.948(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.2284(10)
_cell_length_b                   10.6335(4)
_cell_length_c                   38.1132(13)
_cell_measurement_reflns_used    9150
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      22.8400
_cell_measurement_theta_min      3.5840
_cell_volume                     10527.6(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -20.00  32.00   1.00  120.00    --   -8.54 -99.00-120.00   52
  2  \w    -85.00  24.00   1.00  120.00    --   -8.54 -77.00  30.00  109
  3  \w    -16.00  83.00   1.00  120.00    --    8.62  37.00 -90.00   99
  4  \w    -65.00  37.00   1.00  120.00    --    8.62 -57.00 120.00  102
  5  \w      8.00  70.00   1.00  120.00    --    8.62-135.00  45.00   62
  6  \w    -65.00  37.00   1.00  120.00    --    8.62 -57.00 -60.00  102
  7  \w      7.00  32.00   1.00  120.00    --    8.62-133.00-136.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0255529000
_diffrn_orient_matrix_UB_12      0.0058221000
_diffrn_orient_matrix_UB_13      -0.0039428000
_diffrn_orient_matrix_UB_21      -0.0093413000
_diffrn_orient_matrix_UB_22      -0.0015068000
_diffrn_orient_matrix_UB_23      -0.0183682000
_diffrn_orient_matrix_UB_31      -0.0024371000
_diffrn_orient_matrix_UB_32      0.0664247000
_diffrn_orient_matrix_UB_33      -0.0000813000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1222
_diffrn_reflns_av_unetI/netI     0.0821
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            72777
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.282
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.356
_exptl_crystal_description       needle
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         9285
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+75.6922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6797
_reflns_number_total             9285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02524j2.cif
_cod_data_source_block           hb_47-7_scale_sq
_cod_depositor_comments
'Adding full bibliography for 7046906--7046910.cif.'
_cod_database_code               7046909
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H-Rh2
 1.75 with sigma of 0.05
3.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42),
  C52(H52), C62(H62), C72(H72), C82(H82), C92(H92)
3.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C74(H74A,H74B,H74C), C75(H75A,
 H75B,H75C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C94(H94A,H94B,H94C),
 C95(H95A,H95B,H95C)
;
_shelx_res_checksum              46944
_shelx_fab_checksum              87801
_ins_header
;
TITL HB_47-7_scale in Cc 
REM Cc (#9 in standard setting)
CELL 0.71073  26.228388  10.633546  38.113193  90.0000  97.9481  90.0000
ZERR    8.00   0.001040   0.000361   0.001337   0.0000   0.0036   0.0000
LATT -7
SYMM  x,-y, z+1/2 
SFAC C H B N P Rh
UNIT 392.00 472.00 16.00 96.00 8.00 16.00
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 1.030
_oxdiff_exptl_absorpt_empirical_full_min 0.956