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_7046907
_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         'C57 H62 B2 N8 P2 Rh2, C6 H14'
_chemical_formula_sum            'C63 H76 B2 N8 P2 Rh2'
_chemical_formula_weight         1234.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-28
_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                 99.155(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7605(7)
_cell_length_b                   13.5447(6)
_cell_length_c                   23.3266(10)
_cell_measurement_reflns_used    9445
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.4160
_cell_measurement_theta_min      3.4840
_cell_volume                     5851.9(4)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_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  30.00   1.00    5.00    --  -11.22 -99.00 150.00   50
  2  \w    -39.00  62.00   1.00    5.00    --  -11.22  57.00  60.00  101
  3  \w    -98.00 -34.00   1.00    5.00    --  -11.22 178.00-150.00   64
  4  \w    -86.00  13.00   1.00    5.00    --  -11.22 -37.00 -90.00   99
  5  \w    -63.00  24.00   1.00    5.00    --   11.30 -37.00-150.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0067658000
_diffrn_orient_matrix_UB_12      -0.0131226000
_diffrn_orient_matrix_UB_13      -0.0298224000
_diffrn_orient_matrix_UB_21      -0.0276815000
_diffrn_orient_matrix_UB_22      0.0360999000
_diffrn_orient_matrix_UB_23      -0.0049461000
_diffrn_orient_matrix_UB_31      0.0255697000
_diffrn_orient_matrix_UB_32      0.0356025000
_diffrn_orient_matrix_UB_33      -0.0059310000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30447
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.490
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85241
_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    1.401
_exptl_crystal_description       plate
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.357
_exptl_crystal_size_min          0.241
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+29.6662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4551
_reflns_number_total             5971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02524j2.cif
_cod_data_source_block           hb_76-1_scale
_cod_depositor_comments
'Adding full bibliography for 7046906--7046910.cif.'
_cod_database_code               7046907
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2.a Secondary CH2 refined with riding coordinates:
 C102(H10D,H10E), C103(H10F,H10G)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), 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)
2.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C101(H10A,H10B,H10C)
;
_shelx_res_checksum              25051
_ins_header
;
TITL HB_76-1_scale in I2/a 
REM I2/a (#15 in standard setting)
CELL 0.71073  18.760516  13.544747  23.326639  90.0000  99.1549  90.0000
ZERR    4.00   0.000745   0.000583   0.000990   0.0000   0.0038   0.0000
LATT  2
SYMM -x+1/2, y,-z 
SFAC C H B N P Rh
UNIT 228.00 248.00 8.00 32.00 8.00 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 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.842