Carbide complexes as π-acceptor ligands
Reinholdt, Anders; Vibenholt, Johan E.; Morsing, Thorbjørn J.; Schau-Magnussen, Magnus; Reeler, Nini E. A.; Bendix, Jesper; Chem. Sci. 6 (2015) 5815–; doi:10.1039/C5SC02077H

data_1521279
_publ_section_title
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 Carbide complexes as \p-acceptor ligands
;
_journal_issue                   10
_journal_name_full               'Chem. Sci.'
_journal_page_first              5815
_journal_paper_doi               10.1039/C5SC02077H
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C42 H71 Cl4 N P2 Pt Ru, C H Cl3'
_chemical_formula_sum            'C43 H72 Cl7 N P2 Pt Ru'
_chemical_formula_weight         1209.26
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-26 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                85.8029(11)
_cell_angle_beta                 78.4958(10)
_cell_angle_gamma                76.9593(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6223(3)
_cell_length_b                   14.2389(5)
_cell_length_c                   18.6464(7)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.38
_cell_volume                     2437.81(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30567
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         2.212
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.656
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1059 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.4599.
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    1.647
_exptl_crystal_description       rod
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         11589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0190P)^2^+0.5140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9665
_reflns_number_total             11589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02077h2.cif
_cod_data_source_block           mo_scan_0m-1
_cod_depositor_comments
'Adding full bibliography for 1521279--1521290.cif.'
_cod_database_code               1521279
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.668
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C28A) = Uanis(C28)
Uanis(C30) = Uanis(C30A)
3. Others
 Sof(H25A)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=
 Sof(H29C)=Sof(H29D)=Sof(H27C)=Sof(H27D)=1-FVAR(1)
 Sof(H25)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H29A)=
 Sof(H29B)=Sof(H27A)=Sof(H27B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C37(H37), C13(H13), C25(H25), C25(H25A), C31(H31), C7(H7), C43(H43)
4.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C39(H39A,H39B), C34(H34A,H34B), C32(H32A,
 H32B), C36(H36A,H36B), C12(H12A,H12B), C9(H9A,H9B), C38(H38A,H38B), C11(H11A,
 H11B), C22(H22A,H22B), C17(H17A,H17B), C20(H20A,H20B), C14(H14A,H14B),
 C41(H41A,H41B), C18(H18A,H18B), C10(H10A,H10B), C42(H42A,H42B), C16(H16A,H16B),
  C8(H8A,H8B), C40(H40A,H40B), C33(H33A,H33B), C21(H21A,H21B), C15(H15A,H15B),
 C30(H30A,H30B), C35(H35A,H35B), C28(H28A,H28B), C30A(H30C,H30D), C28A(H28C,
 H28D), C29(H29A,H29B), C29(H29C,H29D), C26(H26A,H26B), C27(H27A,H27B),
 C27(H27C,H27D)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C2(H2), C4(H4), C6(H6)
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_shelx_res_checksum              88469
_olex2_submission_special_instructions 'No special instructions were received'