Synthons for carbide complex chemistry.
Reinholdt, Anders; Hill, Anthony F.; Bendix, Jesper; Chemical communications (Cambridge, England) 54 (2018) 5708–5711; doi:10.1039/c8cc03596b

data_7121652
_publ_section_title
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 Synthons for carbide complex chemistry.
;
_journal_issue                   45
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5708
_journal_page_last               5711
_journal_paper_doi               10.1039/c8cc03596b
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety
'C51 H92 Cl4 P4 Pt Ru, C2 H3 N, 0.5(C N), 0.5(C H3)'
_chemical_formula_sum            'C54 H96.5 Cl4 N1.5 P4 Pt Ru'
_chemical_formula_weight         1328.66
_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
_audit_creation_date             2018-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-02-15 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1342(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6472(6)
_cell_length_b                   19.8469(8)
_cell_length_c                   21.3940(8)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      42.245
_cell_measurement_theta_min      3.027
_cell_volume                     6171.1(4)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            223878
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.728
_diffrn_reflns_theta_min         2.176
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.820
_exptl_absorpt_correction_T_max  0.7489
_exptl_absorpt_correction_T_min  0.6186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0901 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.8260.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             2724
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.111
_refine_diff_density_max         2.412
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         24590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+4.3249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20767
_reflns_number_total             24590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03596b2.cif
_cod_data_source_block           mo_d8v3150_0m-1
_cod_depositor_comments
'Adding full bibliography for 7121645--7121655.cif.'
_cod_original_formula_sum        'C54 H96.50 Cl4 N1.50 P4 Pt Ru'
_cod_database_code               7121652
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.745
_shelx_estimated_absorpt_t_min   0.514
_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. Others
 Fixed Sof: N2(0.5) C55(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
3.a Ternary CH refined with riding coordinates:
 C46(H46), C4(H4), C22(H22), C34(H34), C40(H40), C28(H28), C10(H10), C16(H16)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C39(H39A,H39B), C18(H18A,H18B), C32(H32A,H32B), C43(H43A,H43B),
 C38(H38A,H38B), C41(H41A,H41B), C36(H36A,H36B), C21(H21A,H21B), C26(H26A,H26B),
  C19(H19A,H19B), C42(H42A,H42B), C37(H37A,H37B), C9(H9A,H9B), C29(H29A,H29B),
 C33(H33A,H33B), C25(H25A,H25B), C17(H17A,H17B), C23(H23A,H23B), C5(H5A,H5B),
 C35(H35A,H35B), C48(H48A,H48B), C11(H11A,H11B), C7(H7A,H7B), C20(H20A,H20B),
 C2(H2A,H2B), C51(H51A,H51B), C15(H15A,H15B), C27(H27A,H27B), C30(H30A,H30B),
 C45(H45A,H45B), C6(H6A,H6B), C50(H50A,H50B), C49(H49A,H49B), C14(H14A,H14B),
 C8(H8A,H8B), C24(H24A,H24B), C47(H47A,H47B), C12(H12A,H12B), C31(H31A,H31B),
 C13(H13A,H13B), C44(H44A,H44B)
3.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C)
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_shelx_res_checksum              22596
_olex2_submission_special_instructions 'No special instructions were received'