Dimetalla-heterocyclic carbenes: the interconversion of chalcocarbonyl and carbido ligands.
Barnett, Harrison J.; Hill, Anthony F.; Chemical communications (Cambridge, England) 56 (2020) 12593–12596; doi:10.1039/d0cc05106c

data_7127192
_publ_section_title
;
 Dimetalla-heterocyclic carbenes: the interconversion of chalcocarbonyl
 and carbido ligands.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12593
_journal_page_last               12596
_journal_paper_doi               10.1039/d0cc05106c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C51 H44 Cl2 P4 Rh2 Se, 1.5(C7 H8)'
_chemical_formula_sum            'C61.5 H56 Cl2 P4 Rh2 Se'
_chemical_formula_weight         1274.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-27 deposited with the CCDC.	2020-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                70.671(2)
_cell_angle_beta                 75.071(2)
_cell_angle_gamma                80.200(2)
_cell_formula_units_Z            4
_cell_length_a                   16.2884(4)
_cell_length_b                   20.0388(5)
_cell_length_c                   22.3244(6)
_cell_measurement_reflns_used    12153
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.4300
_cell_measurement_theta_min      4.3130
_cell_volume                     6615.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.962
_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    -84.00 -24.00   1.00    4.00    --  -36.03 125.00  30.00   60
  2  \w    -98.00  23.00   1.00    4.00    --  -36.03   0.00-180.00  121
  3  \w   -105.00 -31.00   1.00    4.00    --  -36.03 -38.00 -30.00   74
  4  \w    -70.00  -6.00   1.00    4.00    --  -36.03 125.00 120.00   64
  5  \w     27.00  86.00   1.00    4.00    --   36.03-125.00 -30.00   59
  6  \w     36.00 109.00   1.00   14.00    --  105.15-111.00 150.00   73
  7  \w     38.00 118.00   1.00   14.00    --  105.15 -45.00   0.00   80
  8  \w     39.00 165.00   1.00   14.00    --  105.15   0.00 -60.00  126
  9  \w     37.00 118.00   1.00   14.00    --  105.15 -45.00-120.00   81
 10  \w     46.00 109.00   1.00   14.00    --  105.15-111.00-120.00   63
 11  \w     44.00 106.00   1.00   14.00    --  105.15 -45.00  90.00   62
 12  \w     49.00 123.00   1.00   14.00    --  105.15 -45.00 150.00   74
 13  \w     50.00 106.00   1.00   14.00    --  105.15 -95.00  30.00   56
 14  \w    115.00 157.00   1.00   14.00    --  105.15  61.00 -60.00   42
 15  \w    103.00 172.00   1.00   14.00    --  105.15  77.00 150.00   69
 16  \w     51.00 123.00   1.00   14.00    --  105.15 -77.00-120.00   72
;
_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      -0.0757209000
_diffrn_orient_matrix_UB_12      -0.0343771000
_diffrn_orient_matrix_UB_13      0.0522842000
_diffrn_orient_matrix_UB_21      -0.0592219000
_diffrn_orient_matrix_UB_22      0.0335693000
_diffrn_orient_matrix_UB_23      -0.0481530000
_diffrn_orient_matrix_UB_31      0.0205994000
_diffrn_orient_matrix_UB_32      -0.0662343000
_diffrn_orient_matrix_UB_33      -0.0236343000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38393
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.863
_diffrn_reflns_theta_min         3.498
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.571
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             2572
_exptl_crystal_preparation       'DCM/Toluene evaporation'
_exptl_crystal_recrystallization_method -
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.066
_refine_diff_density_max         3.324
_refine_diff_density_min         -2.024
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1201
_refine_ls_number_reflns         24534
_refine_ls_number_restraints     459
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0833
_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^)+(0.1503P)^2^+19.4607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2326
_refine_ls_wR_factor_ref         0.2599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18074
_reflns_number_total             24534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05106c2.cif
_cod_data_source_block           hb_1236-3-1a_scale
_cod_depositor_comments
;
Adding full bibliography for 7127189--7127192.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C123 H112 Cl4 P8 Rh4 Se2'
_cod_original_formula_weight         2549.24
_cod_original_formula_moiety         '2(C51 H44 Cl2 P4 Rh2 Se), 3(C7 H8)'
_cod_original_formula_units_Z            2
_cod_database_code               7127192
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C51 H44 Cl2 P4 Rh2 Se1'
_reflns_odcompleteness_completeness 99.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Rigid bond restraints
 C141, C145, C143, C144, C142, C146
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C114, C112, C116, C111, C113, C115
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C216, C220, C217, C218, C219, C221, C215
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C63, C62, C61, C64, C66, C65
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C207, C202, C205, C203, C201, C204, C206
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C214, C212, C209, C213, C211, C210, C208
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C33, C36, C34, C35, C32
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C75, C73, C71, C74, C72, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Uiso/Uaniso restraints and constraints
C141 \\sim C145 \\sim C143 \\sim C144 \\sim C142 \\sim C146: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C114 \\sim C112 \\sim C116 \\sim C111 \\sim C113 \\sim C115: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C216 \\sim C220 \\sim C217 \\sim C218 \\sim C219 \\sim C221 \\sim C215: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C63 \\sim C62 \\sim C61 \\sim C64 \\sim C66 \\sim C65: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C207 \\sim C202 \\sim C205 \\sim C203 \\sim C201 \\sim C204 \\sim C206: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C214 \\sim C212 \\sim C209 \\sim C213 \\sim C211 \\sim C210 \\sim C208: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C31 \\sim C33 \\sim C36 \\sim C34 \\sim C35 \\sim C32: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C75 \\sim C73 \\sim C71 \\sim C74 \\sim C72 \\sim C76: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C6(H6A,H6B), C5(H5A,H5B)
4.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C75(H75), C33(H33), C24(H24), C15(H15), C63(H63), C84(H84),
 C62(H62), C16(H16), C42(H42), C73(H73), C44(H44), C74(H74), C25(H25), C82(H82),
  C36(H36), C64(H64), C86(H86), C83(H83), C12(H12), C34(H34), C66(H66),
 C35(H35), C26(H26), C85(H85), C43(H43), C72(H72), C32(H32), C13(H13), C76(H76),
  C14(H14), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C45(H45),
 C22(H22), C46(H46), C65(H65), C184(H184), C174(H174), C126(H126), C122(H122),
 C123(H123), C124(H124), C125(H125), C165(H165), C133(H133), C176(H176),
 C155(H155), C166(H166), C185(H185), C183(H183), C136(H136), C175(H175),
 C135(H135), C163(H163), C145(H145), C144(H144), C143(H143), C142(H142),
 C146(H146), C132(H132), C164(H164), C153(H153), C152(H152), C182(H182),
 C186(H186), C154(H154), C172(H172), C112(H112), C113(H113), C114(H114),
 C115(H115), C116(H116), C134(H134), C156(H156), C162(H162), C173(H173),
 C214(H214), C213(H213), C212(H212), C211(H211), C210(H210), C217(H217),
 C218(H218), C219(H219), C220(H220), C221(H221), C207(H207), C205(H205),
 C203(H203), C204(H204), C206(H206)
4.c Fitted hexagon refined as free rotating group:
 C51(C52,C53,C54,C55,C56), C126(C121,C122,C123,C124,C125), C145(C144,C143,C142,
 C141,C146), C111(C112,C113,C114,C115,C116), C209(C214,C213,C212,C211,C210),
 C216(C217,C218,C219,C220,C221)
4.d Idealised Me refined as rotating group:
 C208(H20A,H20B,H20C), C215(H21A,H21B,H21C), C201(H20D,H20E,H20F)
;
_shelx_res_checksum              8130
_shelx_fab_checksum              55
_ins_header
;
TITL HB_1236-3-1a_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  16.288417  20.038761  22.324392  70.6712  75.0707  80.2003
ZERR    6.00   0.000383   0.000531   0.000583   0.0024   0.0021   0.0021
LATT  1
SFAC C H P Cl Se Rh
UNIT 306.00 264.00 24.00 12.00 6.00 12.00
TREF
HKLF 4
END
;
_olex2_exptl_crystal_mounting_method -
_olex2_submission_original_sample_id HB_1236_3_1
_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 1.544
_oxdiff_exptl_absorpt_empirical_full_min 0.657