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_7121654
_publ_section_title
;
 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
'C55 H79 Cl2 N3 P2 Pt Ru, 1.33(Cl), 4(C0.33 H0.33 Cl)'
_chemical_formula_sum            'C56.33 H80.33 Cl7.33 N3 P2 Pt Ru'
_chemical_formula_weight         1417.63
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   28.4392(9)
_cell_length_b                   28.4392(9)
_cell_length_c                   13.8884(5)
_cell_measurement_reflns_used    9103
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.110
_cell_measurement_theta_min      2.481
_cell_volume                     9727.9(6)
_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 0.998
_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  0.0482
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            192645
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.210
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.775
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0927 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.8977.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       prism
_exptl_crystal_F_000             4296
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.151
_refine_diff_density_max         1.636
_refine_diff_density_min         -1.590
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         14846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+26.3582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12658
_reflns_number_total             14846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03596b2.cif
_cod_data_source_block           mo_d8v3053_0m-1
_cod_depositor_comments
'Adding full bibliography for 7121645--7121655.cif.'
_cod_original_cell_volume        9727.9(7)
_cod_database_code               7121654
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.679
_shelx_estimated_absorpt_t_min   0.632
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
 Sof(H57A)=Sof(Cl8A)=Sof(Cl7A)=1-FVAR(1)
 Sof(Cl7)=Sof(Cl8)=Sof(H57)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N1(H1), C41(H41), C16(H16), C7(H7), C17(H17), C6(H6), C8(H8), C40(H40),
 C32(H32), C18(H18), C42(H42), C31(H31), C30(H30), C56(H56), C57(H57), C57(H57A)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C43(H43A,H43B), C22(H22A,H22B), C11(H11A,H11B), C5(H5A,H5B),
 C15(H15A,H15B), C19(H19A,H19B), C3(H3A,H3B), C4(H4A,H4B), C24(H24A,H24B),
 C23(H23A,H23B), C20(H20A,H20B), C21(H21A,H21B), C45(H45A,H45B), C9(H9A,H9B),
 C10(H10A,H10B), C33(H33A,H33B), C37(H37A,H37B), C25(H25A,H25B), C14(H14A,H14B),
  C38(H38A,H38B), C39(H39A,H39B), C35(H35A,H35B), C27(H27A,H27B), C29(H29A,
 H29B), C28(H28A,H28B), C34(H34A,H34B), C44(H44A,H44B)
3.c Aromatic/amide H refined with riding coordinates:
 C55(H55), C51(H51), C50(H50), C49(H49), C54(H54), C52(H52), C46(H46),
 C47(H47), C53(H53), C48(H48)
;
_shelx_res_checksum              41613
_olex2_submission_special_instructions 'No special instructions were received'