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_1521282
_publ_section_title
;
 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         'C45 H78 Cl3 Ir P2 Ru, C6 H14'
_chemical_formula_sum            'C51 H92 Cl3 Ir P2 Ru'
_chemical_formula_weight         1166.80
_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   mixed
_audit_creation_date             2015-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 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                111.788(2)
_cell_angle_beta                 96.293(2)
_cell_angle_gamma                99.958(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9458(6)
_cell_length_b                   15.8362(9)
_cell_length_c                   16.7533(10)
_cell_measurement_reflns_used    9725
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.39
_cell_volume                     2607.5(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0585
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            123709
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.112
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.086
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0850 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.8752.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         9185
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+1.7518P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8222
_reflns_number_total             9185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02077h2.cif
_cod_data_source_block           mo_d8v911_0m
_cod_depositor_comments
'Adding full bibliography for 1521279--1521290.cif.'
_cod_database_code               1521282
_shelxl_version_number           2013-2
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C14-C9 \\sim C15-C8
 with sigma of 0.02
 C8-C10 \\sim C9-C11 \\sim C5-C15 \\sim C6-C14
 with sigma of 0.02
 C54-C53 \\sim C58-C59 \\sim C55-C54 \\sim C60-C59 \\sim C60-C61 \\sim C55-C56
 with sigma of 0.02
 C52-C58 \\sim C52-C53 \\sim C56-C57 \\sim C61-C62
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C15)
Uanis(C8) = Uanis(C9)
Uanis(C10) = Uanis(C11)
Uanis(C6) = Uanis(C5)
Uanis(C53) = Uanis(C58)
Uanis(C54) = Uanis(C59)
Uanis(C60) = Uanis(C55)
Uanis(C56) = Uanis(C61)
Uanis(C62) = Uanis(C57)
4. Others
 Sof(H12C)=Sof(H12D)=Sof(H4BC)=Sof(H4BD)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(C8)=Sof(H8)=Sof(C15)=Sof(H15)=1-FVAR(1)
 Sof(H12A)=Sof(H12B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C9)=Sof(H9)=Sof(C14)=
 Sof(H14)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H4AA)=Sof(H4AB)=FVAR(1)
 Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C62)=
 Sof(H62A)=Sof(H62B)=Sof(H62C)=1-FVAR(2)
 Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=
 Sof(H54B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=
 Sof(C56)=Sof(H56A)=Sof(H56B)=FVAR(2)
5.a Riding coordinates:
 C52(H52A,H52B,H52C), C52(H52D,H52E,H52F), C57(H57A,H57B,H57C), C62(H62A,H62B,
 H62C)
5.b Ternary CH refined with riding coordinates:
 C3(H3), C9(H9), C14(H14), C2(H2), C16(H16), C22(H22), C28(H28), C40(H40),
 C46(H46), C34(H34), C8(H8), C15(H15)
5.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C12(H12C,H12D), C11(H11A,H11B), C6(H6A,H6B), C4(H4AA,H4AB),
 C4(H4BC,H4BD), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
  C27(H27A,H27B), C33(H33A,H33B), C32(H32A,H32B), C31(H31A,H31B), C30(H30A,
 H30B), C29(H29A,H29B), C45(H45A,H45B), C44(H44A,H44B), C43(H43A,H43B),
 C42(H42A,H42B), C41(H41A,H41B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B),
  C50(H50A,H50B), C51(H51A,H51B), C39(H39A,H39B), C38(H38A,H38B), C37(H37A,
 H37B), C36(H36A,H36B), C35(H35A,H35B), C53(H53A,H53B), C54(H54A,H54B),
 C55(H55A,H55B), C56(H56A,H56B), C10(H10A,H10B), C5(H5A,H5B), C59(H59A,H59B),
 C58(H58A,H58B), C61(H61A,H61B), C60(H60A,H60B)
;
_shelx_res_checksum              59107