Halogenation of A-frame μ-carbido complexes: a diamagnetic rhodium(ii) carbido complex.
Barnett, Harrison J.; Hill, Anthony F.; Chemical communications (Cambridge, England) 56 (2020) 7738–7740; doi:10.1039/d0cc02349c

data_7126643
_publ_section_title
;
 Halogenation of A-frame \m-carbido complexes: a diamagnetic rhodium(ii)
 carbido complex.
;
_journal_issue                   56
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7738
_journal_page_last               7740
_journal_paper_doi               10.1039/d0cc02349c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '0.5(C69 H56 Cl4 Fe2 P4 Rh2)'
_chemical_formula_sum            'C34.5 H28 Cl2 Fe P2 Rh'
_chemical_formula_weight         734.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-06 deposited with the CCDC.	2020-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.1949(4)
_cell_length_b                   31.0550(6)
_cell_length_c                   40.4621(7)
_cell_measurement_reflns_used    11052
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5780
_cell_measurement_theta_min      4.8930
_cell_volume                     16580.1(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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    -30.00  35.00   1.00    6.00    --   37.06 -57.00 -30.00   65
  2  \w     24.00  90.00   1.00    6.00    --   37.06-125.00 -30.00   66
  3  \w     40.00  76.00   1.00    6.00    --   37.06 -99.00  90.00   36
  4  \w    -29.00  40.00   1.00    6.00    --   37.06 -57.00 120.00   69
  5  \w     21.00  74.00   1.00    6.00    --   37.06  46.00-122.00   53
  6  \w     16.00 108.00   1.00    6.00    --   37.06  19.00 -60.00   92
  7  \w      3.00  31.00   1.00    6.00    --   37.06 -99.00  90.00   28
  8  \w    -30.00  58.00   1.00    6.00    --   37.06 -77.00  30.00   88
  9  \w    123.00 177.00   1.00   20.00    --  111.00  30.00-120.00   54
 10  \w     56.00 108.00   1.00   20.00    --  111.00 -95.00  30.00   52
 11  \w     41.00 110.00   1.00   20.00    --  111.00-111.00   0.00   69
 12  \w     69.00 145.00   1.00   20.00    --  111.00 178.00  30.00   76
 13  \w     86.00 177.00   1.00   20.00    --  111.00  77.00 120.00   91
 14  \w     51.00 129.00   1.00   20.00    --  111.00 -61.00  60.00   78
 15  \w     65.00 107.00   1.00   20.00    --  111.00 -95.00-180.00   42
 16  \w     43.00 126.00   1.00   20.00    --  111.00 -45.00 150.00   83
 17  \w     81.00 109.00   1.00   20.00    --  111.00-111.00 150.00   28
 18  \w     43.00 114.00   1.00   20.00    --  111.00 -45.00 -30.00   71
 19  \w     98.00 178.00   1.00   20.00    --  111.00   0.00-150.00   80
 20  \w     42.00  68.00   1.00   20.00    --  111.00   0.00-150.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0926189000
_diffrn_orient_matrix_UB_12      -0.0137215000
_diffrn_orient_matrix_UB_13      -0.0205890000
_diffrn_orient_matrix_UB_21      -0.0257383000
_diffrn_orient_matrix_UB_22      -0.0476787000
_diffrn_orient_matrix_UB_23      0.0063665000
_diffrn_orient_matrix_UB_31      -0.0660267000
_diffrn_orient_matrix_UB_32      -0.0006580000
_diffrn_orient_matrix_UB_33      -0.0314312000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            22852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.761
_diffrn_reflns_theta_min         3.800
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       dark
_exptl_crystal_F_000             5920
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.391
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0911P)^2^+49.5835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3806
_reflns_number_total             4177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02349c3.cif
_cod_data_source_block           hb_1049-1_scale
_cod_depositor_comments
'Adding full bibliography for 7126642--7126643.cif.'
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C34.50 H28 Cl2 Fe P2 Rh'
_cod_database_code               7126643
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C006(H006), C009(H009), C00A(H00A), C00B(H00B), C00C(H00C), C00D(H00D),
 C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00J(H00J), C00K(H00K),
 C00L(H00L), C00M(H00M)
;
_shelx_res_checksum              26462
_shelx_hkl_checksum              66003
_shelx_fab_checksum              7211
_ins_header
;
TITL HB_1049-1_scale in Fddd 
REM Fddd (#70 in standard setting)
CELL 1.54184  13.194881  31.055039  40.462129  90.0000  90.0000  90.0000
ZERR   15.00   0.000411   0.000566   0.000690   0.0000   0.0000   0.0000
LATT  4
SYMM -x+3/4,-y+3/4, z 
SYMM -x+3/4, y,-z+3/4 
SYMM  x,-y+3/4,-z+3/4 
SFAC C H P Cl Fe Rh
UNIT 750.00 600.00 60.00 60.00 30.00 30.00
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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.203
_oxdiff_exptl_absorpt_empirical_full_min 0.565