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_1521281
_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
'C75 H132 Cl5 Ir O P4 Ru2, 2(C H Cl3), C4 H10 O'
_chemical_formula_sum            'C81 H144 Cl11 Ir O2 P4 Ru2'
_chemical_formula_weight         2058.12
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 97.877(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8110(18)
_cell_length_b                   40.893(6)
_cell_length_c                   16.343(2)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    122.4
_cell_measurement_theta_max      27.698
_cell_measurement_theta_min      2.349
_cell_volume                     9143(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      122.4
_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  0.1059
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            71347
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.135
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.212
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.0787 before and 0.0708 after correction. The Ratio of minimum to maximum transmission is 0.9335. 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    1.495
_exptl_crystal_description       prism
_exptl_crystal_F_000             4232
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         9355
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0346
_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^+26.3160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7077
_reflns_number_total             9355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02077h2.cif
_cod_data_source_block           mo_d8v742_0m-1
_cod_depositor_comments
'Adding full bibliography for 1521279--1521290.cif.'
_cod_database_code               1521281
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.677
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
Uanis(C19A) \\sim Ueq, Uanis(C17A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.2
3. Others
 Sof(H18C)=Sof(H18D)=Sof(H16A)=Sof(H20C)=Sof(H20D)=Sof(C17A)=Sof(H17C)=
 Sof(H17D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(H16)=Sof(H20A)=Sof(H20B)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=FVAR(1)
 Fixed Sof: Cl1(0.5) C3(0.5) O1(0.5)
4.a Ternary CH refined with riding coordinates:
 C4(H4), C10(H10), C40(H40), C28(H28), C16(H16), C16(H16A), C22(H22), C34(H34)
4.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C7(H7A,H7B), C15(H15A,H15B), C31(H31A,H31B), C30(H30A,H30B),
 C25(H25A,H25B), C29(H29A,H29B), C5(H5A,H5B), C26(H26A,H26B), C38(H38A,H38B),
 C9(H9A,H9B), C18(H18A,H18B), C18(H18C,H18D), C36(H36A,H36B), C11(H11A,H11B),
 C27(H27A,H27B), C6(H6A,H6B), C37(H37A,H37B), C35(H35A,H35B), C8(H8A,H8B),
 C33(H33A,H33B), C39(H39A,H39B), C12(H12A,H12B), C20(H20A,H20B), C20(H20C,H20D),
  C24(H24A,H24B), C21(H21A,H21B), C32(H32A,H32B), C14(H14A,H14B), C19(H19A,
 H19B), C17(H17A,H17B), C13(H13A,H13B), C41(H41A,H41B), C17A(H17C,H17D),
 C19A(H19C,H19D)
4.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C)
;
_shelx_res_checksum              37078
_olex2_submission_special_instructions 'No special instructions were received'