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_7126642
_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         'C69 H56 Cl2 Fe2 P4 Rh2, 2(C H2 Cl2)'
_chemical_formula_sum            'C71 H60 Cl6 Fe2 P4 Rh2'
_chemical_formula_weight         1567.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-09-15 deposited with the CCDC.	2020-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.747(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1742(3)
_cell_length_b                   26.8362(6)
_cell_length_c                   18.2963(3)
_cell_measurement_reflns_used    22265
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.1970
_cell_measurement_theta_min      3.5250
_cell_volume                     6468.0(2)
_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      150.01(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    -39.00  62.00   1.00   40.00    --  -11.22  57.00  60.00  101
  2  \w    -20.00  30.00   1.00   40.00    --  -11.22 -99.00 120.00   50
  3  \w    -39.00  62.00   1.00   40.00    --  -11.22  57.00-120.00  101
  4  \w    -98.00 -34.00   1.00   40.00    --  -11.22 178.00-150.00   64
  5  \w    -52.00  69.00   1.00   40.00    --  -11.22  19.00-180.00  121
  6  \w    -39.00  62.00   1.00   40.00    --  -11.22  57.00 -30.00  101
  7  \w    -20.00  30.00   1.00   40.00    --  -11.22 -99.00-150.00   50
  8  \w    -20.00  30.00   1.00   40.00    --  -11.22 -99.00 -30.00   50
  9  \w    -83.00  -4.00   1.00   40.00    --  -11.22 -57.00 120.00   79
 10  \w    -20.00  30.00   1.00   40.00    --  -11.22 -99.00  30.00   50
;
_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      0.0535038000
_diffrn_orient_matrix_UB_12      0.0016060000
_diffrn_orient_matrix_UB_13      0.0042168000
_diffrn_orient_matrix_UB_21      0.0049852000
_diffrn_orient_matrix_UB_22      -0.0243345000
_diffrn_orient_matrix_UB_23      -0.0146749000
_diffrn_orient_matrix_UB_31      0.0035074000
_diffrn_orient_matrix_UB_32      0.0102065000
_diffrn_orient_matrix_UB_33      -0.0356233000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            131471
_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         3.361
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.331
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92028
_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    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         13206
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+18.5762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10044
_reflns_number_total             13206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02349c3.cif
_cod_data_source_block           hb_1015_1_scale
_cod_depositor_comments
'Adding full bibliography for 7126642--7126643.cif.'
_cod_database_code               7126642
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.74
_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
2. Uiso/Uaniso restraints and constraints
Cl21 \\sim Cl22 \\sim C121: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.04
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
 Sof(Cl32)=Sof(Cl31)=Sof(C122)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(Cl21)=Sof(Cl22)=Sof(C121)=Sof(H12A)=Sof(H12B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C111(H11A,H11B), C121(H12A,H12B), C122(H12C,H12D)
4.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), C58(H58), C59(H59), C60(H60), 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), C101(H101), C103(H103), C104(H104), C105(H105),
 C107(H107), C108(H108), C109(H109), C110(H110)
;
_shelx_res_checksum              69332
_shelx_hkl_checksum              57106
_ins_header
;
TITL HB_1015_1_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  13.174193  26.836214  18.296303  90.0000  90.7475  90.0000
ZERR    4.00   0.000297   0.000596   0.000328   0.0000   0.0019   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H P Cl Fe Rh
UNIT 276.00 224.00 16.00 8.00 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 1.169
_oxdiff_exptl_absorpt_empirical_full_min 0.894