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_7046908
_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         'C55 H50 B2 N12 P2 Rh2'
_chemical_formula_sum            'C55 H50 B2 N12 P2 Rh2'
_chemical_formula_weight         1168.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-04-03 deposited with the CCDC.
2018-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.8404(3)
_cell_length_b                   13.2630(2)
_cell_length_c                   11.7030(2)
_cell_measurement_reflns_used    23645
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.4260
_cell_measurement_theta_min      3.6460
_cell_volume                     2924.35(8)
_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      150.00(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 0.901
_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    -86.00  13.00   1.00   60.00    --  -11.22 -37.00 150.00   99
  2  \w    -20.00  30.00   1.00   60.00    --  -11.22 -99.00  90.00   50
  3  \w    -37.00  62.00   1.00   60.00    --  -11.22  43.00 -63.00   99
  4  \w    -61.00  39.00   1.00   60.00    --   11.30 -57.00 -30.00  100
  5  \w    -17.00  84.00   1.00   60.00    --   11.30  57.00 120.00  101
  6  \w    -20.00  41.00   1.00   60.00    --   11.30 -99.00  90.00   61
  7  \w    -63.00  36.00   1.00   60.00    --   11.30 -37.00 120.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0152673000
_diffrn_orient_matrix_UB_12      0.0404095000
_diffrn_orient_matrix_UB_13      0.0312014000
_diffrn_orient_matrix_UB_21      -0.0132775000
_diffrn_orient_matrix_UB_22      0.0209008000
_diffrn_orient_matrix_UB_23      -0.0515273000
_diffrn_orient_matrix_UB_31      -0.0317574000
_diffrn_orient_matrix_UB_32      -0.0281274000
_diffrn_orient_matrix_UB_33      0.0065016000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52285
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.121
_diffrn_reflns_theta_min         3.257
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95090
_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    1.327
_exptl_crystal_description       plate
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 2789 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.023(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         7607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0153P)^2^+1.7862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0552
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.854
_reflns_number_gt                6900
_reflns_number_total             7607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02524j2.cif
_cod_data_source_block           HB_46-3-3
_cod_depositor_comments
'Adding full bibliography for 7046906--7046910.cif.'
_cod_database_code               7046908
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46)
;
_shelx_res_checksum              48070
_shelx_fab_checksum              14081
_ins_header
;
TITL HB_46-3-3_scale in P2(1)2(1)2 
REM P2(1)2(1)2 (#18, found as P22(1)2(1) in -cba setting)
CELL 0.71073  18.840412  13.262995  11.702965  90.0000  90.0000  90.0000
ZERR    2.00   0.000310   0.000247   0.000197   0.0000   0.0000   0.0000
LATT -1
SYMM -x,-y, z 
SYMM -x+1/2, y+1/2,-z 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H B N P Rh
UNIT 110.00 100.00 4.00 24.00 4.00 4.00
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 1.127
_oxdiff_exptl_absorpt_empirical_full_min 0.903