Halogenation of A-Frame μ-Carbido Complexes: Synthesis of η2-Halocarbynes
Hill, Anthony; Barnett, Harrison J.; Chemical Communications  (2019) –; doi:10.1039/C8CC09692A

data_7122810
_publ_section_title
;
 Halogenation of A-Frame \m-Carbido Complexes: Synthesis of
 \h2-Halocarbynes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09692A
_journal_year                    2019
_chemical_formula_moiety         'C55 H50 N2 P4 Rh2, 2(C F3 O3 S), 2(C7 H8)'
_chemical_formula_sum            'C71 H66 F6 N2 O6 P4 Rh2 S2'
_chemical_formula_weight         1551.07
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-07 deposited with the CCDC.
2019-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.506(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7284(3)
_cell_length_b                   23.9123(7)
_cell_length_c                   12.0420(3)
_cell_measurement_reflns_used    7835
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6470
_cell_measurement_theta_min      4.1770
_cell_volume                     3370.89(16)
_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 0.998
_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    -27.00  51.00   1.00    1.00    --   37.21 -38.00 150.00   78
  2  \w     26.00  88.00   1.00    1.00    --   37.21-125.00-180.00   62
  3  \w      8.00  75.00   1.00    1.00    --   37.21 -99.00   0.00   67
  4  \w     21.00 104.00   1.00    1.00    --   37.21  57.00  90.00   83
  5  \w     21.00  98.00   1.00    1.00    --   37.21  57.00  30.00   77
  6  \w      1.00  72.00   1.00    1.00    --   37.21 -99.00 -90.00   71
  7  \w     35.00 105.00   1.00    1.00    --   37.21   0.00-180.00   70
  8  \w    -28.00  30.00   1.00    1.00    --   37.21   0.00-180.00   58
  9  \w     64.00 113.00   1.00    5.00    --  111.00-111.00 -90.00   49
 10  \w     54.00 149.00   1.00    5.00    --  111.00 -15.00   0.00   95
 11  \w     43.00 115.00   1.00    5.00    --  111.00 -45.00 -60.00   72
 12  \w     43.00 127.00   1.00    5.00    --  111.00 -77.00 -90.00   84
 13  \w     41.00 113.00   1.00    5.00    --  111.00-111.00  90.00   72
 14  \w     41.00 118.00   1.00    5.00    --  111.00 -30.00-150.00   77
 15  \w     42.00 107.00   1.00    5.00    --  111.00 -95.00 150.00   65
 16  \w    124.00 178.00   1.00    5.00    --  111.00  61.00-150.00   54
 17  \w     41.00 131.00   1.00    5.00    --  111.00 -30.00 120.00   90
 18  \w     44.00 127.00   1.00    5.00    --  111.00 -61.00  60.00   83
 19  \w     51.00 115.00   1.00    5.00    --  111.00 -61.00 150.00   64
 20  \w     84.00 148.00   1.00    5.00    --  111.00 -15.00-120.00   64
;
_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      -0.1003355000
_diffrn_orient_matrix_UB_12      -0.0143008000
_diffrn_orient_matrix_UB_13      -0.0836141000
_diffrn_orient_matrix_UB_21      -0.0064689000
_diffrn_orient_matrix_UB_22      0.0616311000
_diffrn_orient_matrix_UB_23      -0.0371028000
_diffrn_orient_matrix_UB_31      0.0846677000
_diffrn_orient_matrix_UB_32      -0.0121659000
_diffrn_orient_matrix_UB_33      -0.0899748000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18965
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.776
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.031
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_correction_T_min  0.319
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       needle
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.068
_refine_diff_density_max         2.881
_refine_diff_density_min         -1.608
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         5951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1521P)^2^+32.2780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2618
_refine_ls_wR_factor_ref         0.2702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5146
_reflns_number_total             5951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09692a2.cif
_cod_data_source_block           hb_1046-1_scale
_cod_database_code               7122810
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
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), C102(H102), C103(H103),
 C104(H104), C105(H105), C106(H106)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C107(H10A,H10B,H10C)
;
_shelx_res_checksum              44514
_shelx_hkl_checksum              34598
_ins_header
;
TITL HB_1046-1_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  11.728403  23.912312  12.042005  90.0000  93.5056  90.0000
ZERR    4.00   0.000286   0.000698   0.000344   0.0000   0.0026   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H O F P S Rh
UNIT 160.00 160.00 12.00 12.00 16.00 4.00 8.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.980
_oxdiff_exptl_absorpt_empirical_full_min 0.638