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_7121655
_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 H44 Cl4 P4 Pt Ru, 0.62(C H2 Cl2), C2 H3 N, 0.38(C4 H10 O)'
_chemical_formula_sum            'C55.16 H52.08 Cl5.23 N O0.38 P4 Pt Ru'
_chemical_formula_weight         1340.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                72.0661(15)
_cell_angle_beta                 72.0477(15)
_cell_angle_gamma                63.5052(14)
_cell_formula_units_Z            2
_cell_length_a                   13.1006(5)
_cell_length_b                   13.1671(6)
_cell_length_c                   18.1048(8)
_cell_measurement_reflns_used    9403
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.619
_cell_measurement_theta_min      2.414
_cell_volume                     2605.1(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            145623
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         2.328
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.403
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0889 before and 0.0607 after correction.
The Ratio of minimum to maximum transmission is 0.8244.
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    1.709
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.481
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         14590
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0089P)^2^+5.3785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13763
_reflns_number_total             14590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03596b2.cif
_cod_data_source_block           mo_d8v2038_0m-tri
_cod_depositor_comments
'Adding full bibliography for 7121645--7121655.cif.'
_cod_database_code               7121655
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.662
_shelx_estimated_absorpt_t_min   0.451
_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. Restrained distances
 C55-C56 \\sim C57-C58
 with sigma of 0.001
 O1-C55 \\sim O1-C57
 with sigma of 0.001
 O1-C58 \\sim O1-C56
 with sigma of 0.001
3. Others
 Sof(O1)=Sof(C58)=Sof(H58a)=Sof(H58b)=Sof(H58c)=Sof(C56)=Sof(H56a)=Sof(H56b)=
 Sof(H56c)=Sof(C55)=Sof(H55a)=Sof(H55b)=Sof(C57)=Sof(H57a)=Sof(H57b)=1-FVAR(1)
 Sof(Cl6)=Sof(Cl5)=Sof(C54)=Sof(H54a)=Sof(H54b)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b), C54(H54a,H54b), C55(H55a,H55b), C57(H57a,H57b)
4.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C50(H50), C20(H20), C12(H12), C21(H21), C45(H45), C42(H42),
 C38(H38), C43(H43), C18(H18), C7(H7), C9(H9), C14(H14), C11(H11), C47(H47),
 C41(H41), C44(H44), C39(H39), C15(H15), C8(H8), C19(H19), C33(H33), C30(H30),
 C48(H48), C51(H51), C23(H23), C32(H32), C25(H25), C24(H24), C29(H29), C5(H5),
 C13(H13), C36(H36), C31(H31), C17(H17), C37(H37), C6(H6), C35(H35), C27(H27),
 C26(H26)
4.c Idealised Me refined as rotating group:
 C53(H53a,H53b,H53c), C58(H58a,H58b,H58c), C56(H56a,H56b,H56c)
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_shelx_res_checksum              1346
_olex2_submission_special_instructions 'No special instructions were received'