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_7046906
_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         'C73 H60 Cl2 P4 Rh2, C H2 Cl2'
_chemical_formula_sum            'C74 H62 Cl4 P4 Rh2'
_chemical_formula_weight         1422.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-08
_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                85.461(2)
_cell_angle_beta                 84.2380(10)
_cell_angle_gamma                75.2850(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5983(2)
_cell_length_b                   13.8742(3)
_cell_length_c                   20.5650(4)
_cell_measurement_reflns_used    29219
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6300
_cell_measurement_theta_min      3.8500
_cell_volume                     3453.74(12)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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    -64.00 -30.00   1.00    1.00    --  -37.04  77.00-120.00   34
  2  \w     -3.00  30.00   1.00    1.00    --  -37.04  77.00-120.00   33
  3  \w     65.00  90.00   1.00    1.00    --   37.04  57.00   0.00   25
  4  \w     58.00  85.00   1.00    1.00    --   37.04  38.00  60.00   27
  5  \w     47.00  74.00   1.00    1.00    --   37.04  38.00 -30.00   27
  6  \w     35.00 103.00   1.00    1.00    --   37.04  57.00  60.00   68
  7  \w    139.00 166.00   1.00    1.00    --  111.00  50.00 -30.00   27
  8  \w    133.00 160.00   1.00    1.00    --  111.00  50.00   0.00   27
  9  \w    116.00 149.00   1.00    1.00    --  111.00  64.00 -60.00   33
 10  \w    124.00 151.00   1.00    1.00    --  111.00 111.00 -30.00   27
 11  \w    111.00 141.00   1.00    1.00    --  111.00  50.00 -60.00   30
 12  \w    106.00 133.00   1.00    1.00    --  111.00  38.00 -60.00   27
 13  \w     95.00 127.00   1.00    1.00    --  111.00  50.00   0.00   32
 14  \w    105.00 177.00   1.00    1.00    --  111.00  38.00  30.00   72
 15  \w    121.00 162.00   1.00    1.00    --  111.00  89.00 100.00   41
 16  \w     95.00 153.00   1.00    1.00    --  111.00  50.00  90.00   58
 17  \w    111.00 136.00   1.00    1.00    --  111.00 -25.00   0.00   25
 18  \w     95.00 126.00   1.00    1.00    --  111.00 -64.00 -30.00   31
 19  \w    106.00 133.00   1.00    1.00    --  111.00 -77.00  30.00   27
 20  \w    104.00 146.00   1.00    1.00    --  111.00 -92.00  60.00   42
 21  \w     92.00 119.00   1.00    1.00    --  111.00 -25.00  30.00   27
 22  \w     83.00 127.00   1.00    1.00    --  111.00 -50.00  60.00   44
 23  \w     80.00 113.00   1.00    1.00    --  111.00-111.00 120.00   33
 24  \w     75.00 115.00   1.00    1.00    --  111.00-111.00  60.00   40
 25  \w     81.00 106.00   1.00    1.00    --  111.00-111.00  30.00   25
 26  \w     74.00 114.00   1.00    1.00    --  111.00-111.00   0.00   40
 27  \w     90.00 116.00   1.00    1.00    --  111.00-111.00 -60.00   26
 28  \w     90.00 123.00   1.00    1.00    --  111.00 -92.00 -90.00   33
 29  \w     90.00 127.00   1.00    1.00    --  111.00 -56.00 -61.06   37
 30  \w     86.00 113.00   1.00    1.00    --  111.00-111.00 -90.00   27
 31  \w     84.00 110.00   1.00    1.00    --  111.00-111.00-120.00   26
 32  \w    103.00 136.00   1.00    1.00    --  111.00 -77.00-150.00   33
 33  \w     89.00 116.00   1.00    1.00    --  111.00-111.00-180.00   27
 34  \w     90.00 117.00   1.00    1.00    --  111.00 -64.00-150.00   27
 35  \w     94.00 130.00   1.00    1.00    --  111.00 -38.00-180.00   36
 36  \w     80.00 123.00   1.00    1.00    --  111.00 -12.00 -60.00   43
 37  \w     94.00 131.00   1.00    1.00    --  111.00  50.00-150.00   37
 38  \w     92.00 149.00   1.00    1.00    --  111.00  64.00-150.00   57
 39  \w    138.00 165.00   1.00    1.00    --  111.00 111.00-150.00   27
 40  \w    111.00 144.00   1.00    1.00    --  111.00 178.00 -60.00   33
 41  \w     92.00 123.00   1.00    1.00    --  111.00  77.00  90.00   31
 42  \w     88.00 155.00   1.00    1.00    --  111.00  25.00  90.00   67
 43  \w     90.00 118.00   1.00    1.00    --  111.00 -60.00 178.82   28
 44  \w     81.00 127.00   1.00    1.00    --  111.00 -32.00 129.67   46
 45  \w     79.00 104.00   1.00    1.00    --  111.00 -77.00 120.00   25
 46  \w     69.00 144.00   1.00    1.00    --  111.00 -12.00 150.00   75
 47  \w     76.00 110.00   1.00    1.00    --  111.00  12.00  30.00   34
 48  \w     53.00 127.00   1.00    1.00    --  111.00 -38.00  30.00   74
 49  \w     75.00 102.00   1.00    1.00    --  111.00 -74.00 -33.59   27
 50  \w     59.00 121.00   1.00    1.00    --  111.00 -50.00-120.00   62
 51  \w     49.00  78.00   1.00    1.00    --  111.00 -77.00   0.00   29
 52  \w     53.00  78.00   1.00    1.00    --  111.00 -92.00  60.00   25
 53  \w     47.00 108.00   1.00    1.00    --  111.00 -64.00  60.00   61
 54  \w     42.00  71.00   1.00    1.00    --  111.00-111.00 -60.00   29
 55  \w     42.00  69.00   1.00    1.00    --  111.00 -92.00 -90.00   27
 56  \w     44.00  80.00   1.00    1.00    --  111.00 -56.00 -61.06   36
 57  \w     44.00 129.00   1.00    1.00    --  111.00 -38.00 -60.00   85
 58  \w     65.00  90.00   1.00    1.00    --   37.04-125.00   0.00   25
 59  \w     48.00  81.00   1.00    1.00    --   37.04-125.00  90.00   33
 60  \w     34.00  61.00   1.00    1.00    --   37.04-125.00   0.00   27
 61  \w     45.00  74.00   1.00    1.00    --   37.04 -99.00 -30.00   29
 62  \w     27.00  59.00   1.00    1.00    --   37.04 -89.00 -15.00   32
 63  \w     25.00  63.00   1.00    1.00    --   37.04-125.00 -60.00   38
 64  \w     50.00  75.00   1.00    1.00    --   37.04 -99.00-120.00   25
 65  \w     23.00  80.00   1.00    1.00    --   37.04-125.00-120.00   57
 66  \w     20.00  45.00   1.00    1.00    --   37.04 -57.00-180.00   25
 67  \w    -28.00  -1.00   1.00    1.00    --   37.04 -57.00-180.00   27
 68  \w    -29.00  49.00   1.00    1.00    --   37.04 -57.00-150.00   78
 69  \w     19.00  58.00   1.00    1.00    --   37.04 -19.00 -30.00   39
 70  \w     11.00  65.00   1.00    1.00    --   37.04 -19.00  60.00   54
 71  \w     19.00  75.00   1.00    1.00    --   37.04 -99.00 150.00   56
 72  \w     10.00  37.00   1.00    1.00    --   37.04 -57.00  60.00   27
 73  \w      8.00  50.00   1.00    1.00    --   37.04 -57.00 120.00   42
 74  \w     -3.00  22.00   1.00    1.00    --   37.04 -89.00 -15.00   25
 75  \w    -30.00  14.00   1.00    1.00    --   37.04 -57.00  90.00   44
 76  \w    -31.00  -4.00   1.00    1.00    --   37.04 -19.00 -30.00   27
 77  \w     20.00  62.00   1.00    1.00    --   37.04  57.00   0.00   42
 78  \w     50.00 101.00   1.00    1.00    --  111.00 -12.00  60.00   51
 79  \w     47.00  73.00   1.00    1.00    --  111.00 -77.00 150.00   26
 80  \w     42.00 100.00   1.00    1.00    --  111.00 -25.00  90.00   58
 81  \w     44.00  76.00   1.00    1.00    --  111.00 -77.00-150.00   32
 82  \w     56.00  86.00   1.00    1.00    --  111.00 -50.00-180.00   30
 83  \w     45.00 133.00   1.00    1.00    --  111.00 -77.00-180.00   88
 84  \w     58.00  85.00   1.00    1.00    --  111.00 178.00  90.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0203736000
_diffrn_orient_matrix_UB_12      0.0799970000
_diffrn_orient_matrix_UB_13      0.0507828000
_diffrn_orient_matrix_UB_21      0.0752150000
_diffrn_orient_matrix_UB_22      -0.0743422000
_diffrn_orient_matrix_UB_23      0.0456858000
_diffrn_orient_matrix_UB_31      0.1001192000
_diffrn_orient_matrix_UB_32      0.0359796000
_diffrn_orient_matrix_UB_33      -0.0319455000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53961
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.835
_diffrn_reflns_theta_min         2.163
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70629
_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    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.414
_refine_diff_density_min         -1.358
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         13963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+4.0595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12988
_reflns_number_total             13963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02524j2.cif
_cod_data_source_block           HB_3-1-1_scale_sq
_cod_depositor_comments
'Adding full bibliography for 7046906--7046910.cif.'
_cod_database_code               7046906
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 98.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B)
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), C43(H43), C44(H44), C45(H45), C46(H46), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
  C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C82(H82), C83(H83),
 C84(H84), C85(H85), C86(H86), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96),
  C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C122(H122), C123(H123),
 C124(H124), C125(H125), C126(H126)
;
_shelx_res_checksum              3146
_shelx_fab_checksum              91061
_ins_header
;
TITL HB_3-1-1_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  12.598293  13.874246  20.564976  85.4608  84.2381  75.2847
ZERR    2.00   0.000185   0.000254   0.000394   0.0015   0.0014   0.0014
LATT  1
SFAC C H P Cl Rh
UNIT 146.00 120.00 8.00 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 1.388
_oxdiff_exptl_absorpt_empirical_full_min 0.807