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_7046910
_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 H46 B2 N8 P2 Rh2, 1.25(C H2 Cl2)'
_chemical_formula_sum            'C50.25 H48.5 B2 Cl2.5 N8 P2 Rh2'
_chemical_formula_weight         1142.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-09
_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                 97.097(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.9780(5)
_cell_length_b                   18.6930(2)
_cell_length_c                   23.8266(4)
_cell_measurement_reflns_used    51883
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.4200
_cell_measurement_theta_min      3.4440
_cell_volume                     10597.8(3)
_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 0.998
_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  30.00   1.00   50.00    --  -11.22 -99.00-180.00   50
  2  \w    -39.00  62.00   1.00   50.00    --  -11.22  57.00 -30.00  101
  3  \w    -83.00  17.00   1.00   50.00    --  -11.22 -57.00-180.00  100
  4  \w    -20.00  30.00   1.00   50.00    --  -11.22 -99.00 -30.00   50
  5  \w    -36.00  63.00   1.00   50.00    --  -11.22  37.00  90.00   99
  6  \w    -44.00  65.00   1.00   50.00    --  -11.22  77.00 -30.00  109
  7  \w     34.00  98.00   1.00   50.00    --   11.30-178.00-150.00   64
  8  \w    -20.00  27.00   1.00   50.00    --   11.30 -99.00-120.00   47
;
_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      -0.0238650000
_diffrn_orient_matrix_UB_12      0.0043717000
_diffrn_orient_matrix_UB_13      -0.0204720000
_diffrn_orient_matrix_UB_21      0.0173687000
_diffrn_orient_matrix_UB_22      -0.0031570000
_diffrn_orient_matrix_UB_23      -0.0219089000
_diffrn_orient_matrix_UB_31      -0.0042277000
_diffrn_orient_matrix_UB_32      -0.0375618000
_diffrn_orient_matrix_UB_33      -0.0005299000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            171095
_diffrn_reflns_point_group_measured_fraction_full 0.998
_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         3.265
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90873
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       plate
_exptl_crystal_F_000             4628
_exptl_crystal_size_max          0.645
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.169
_refine_diff_density_max         2.640
_refine_diff_density_min         -1.499
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1185
_refine_ls_number_reflns         21633
_refine_ls_number_restraints     269
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0865
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+148.0331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17224
_reflns_number_total             21633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02524j2.cif
_cod_data_source_block           hb_67-3_scale
_cod_depositor_comments
'Adding full bibliography for 7046906--7046910.cif.'
_cod_original_formula_sum        'C50.25 H48.50 B2 Cl2.50 N8 P2 Rh2'
_cod_database_code               7046910
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.610
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H) groups, All C(H) groups, All C(H,H) groups
2. Restrained distances
 C201-Cl2
 1.6 with sigma of 0.04
 Cl32-C204
 1.6 with sigma of 0.03
3. Rigid bond restraints
 C64, C62, C61, C66, C65, C63
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C106, C101, C102, C103, C104, C105
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C116, C111, C112
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C151, C156, C155, C154, C153, C152
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C132, C136, C133, C134, C135, C131
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C64 \\sim C65 \\sim C66 \\sim C61 \\sim C62 \\sim C63: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Cl1 \\sim Cl2 \\sim C201: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Cl31 \\sim C204 \\sim Cl32: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C106) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C104) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C116) \\sim Ueq, Uanis(C112) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.05
Uanis(C114) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C115) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C201) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C131) \\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C135) \\sim Ueq,
Uanis(C134) \\sim Ueq, Uanis(C133) \\sim Ueq, Uanis(C132) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl31) \\sim Ueq, Uanis(Cl32) \\sim Ueq, Uanis(C204) \\sim Ueq, : with
sigma of 0.05 and sigma for terminal atoms of 0.1
5. Rigid body (RIGU) restrains
 Cl1, Cl2, C201
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C153, C152, C151, C156, C155, C154
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl32, C204, Cl31, H20C, H20D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl32(0.5) Cl31(0.5) C204(0.5) H20C(0.5) H20D(0.5) Cl2(0.5)
 Cl1(0.5) C201(0.5) H20E(0.5) H20F(0.5) Cl21(0.5) Cl22(0.5) C203(0.5) H20G(0.5)
 H20H(0.5)
7.a Secondary CH2 refined with riding coordinates:
 B1(H1A,H1B), B2(H2A,H2B), B3(H3A,H3B), B4(H4A,H4B), C204(H20C,H20D),
 C202(H20A,H20B), C201(H20E,H20F), C203(H20G,H20H)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C41(H41), C121(H121), C12(H12), C122(H122), C42(H42), C81(H81),
 C43(H43), C8AA(H8AA), C16(H16), C3AA(H3AA), C36(H36), C83(H83), C46(H46),
 C6(H6), C92(H92), C86(H86), C93(H93), C72(H72), C82(H82), C123(H123),
 C4AA(H4AA), C84(H84), C22(H22), C94(H94), C85(H85), C7(H7), C96(H96), C44(H44),
  C26(H26), C13(H13), C15(H15), C52(H52), C14(H14), C45(H45), C34(H34),
 C56(H56), C33(H33), C32(H32), C125(H125), C25(H25), C95(H95), C73(H73),
 C124(H124), C35(H35), C24(H24), C126(H126), C23(H23), C54(H54), C74(H74),
 C142(H142), C76(H76), C55(H55), C146(H146), C145(H145), C53(H53), C75(H75),
 C144(H144), C143(H143), C155(H155), C154(H154), C153(H153), C152(H152),
 C156(H156), C105(H105), C106(H106), C102(H102), C103(H103), C104(H104),
 C63(H63), C64(H64), C65(H65), C66(H66), C62(H62), C113(H113), C114(H114),
 C115(H115), C116(H116), C112(H112), C134(H134), C133(H133), C132(H132),
 C136(H136), C135(H135)
7.c Fitted hexagon refined as free rotating group:
 C155(C154,C153,C152,C151,C156), C105(C106,C101,C102,C103,C104), C63(C64,C65,
 C66,C61,C62), C113(C114,C115,C116,C111,C112), C134(C133,C132,C131,C136,C135)
;
_shelx_res_checksum              48904
_ins_header
;
TITL HB_67-3_scale in P2/c 
REM P2/c (#13 in standard setting)
CELL 0.71073  23.977975  18.692969  23.826558  90.0000  97.0970  90.0000
ZERR    8.00   0.000490   0.000245   0.000377   0.0000   0.0017   0.0000
LATT  1
SYMM -x, y,-z+1/2 
SFAC C H B N P Rh
UNIT 392.00 368.00 16.00 64.00 16.00 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 1.140
_oxdiff_exptl_absorpt_empirical_full_min 0.908