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_1521280
_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         'C37 H66 Cl5 P2 Pd Ru, C36 H30 N P2'
_chemical_formula_sum            'C73 H96 Cl5 N P4 Pd Ru'
_chemical_formula_weight         1496.10
_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             2015-05-24
_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                76.202(4)
_cell_angle_beta                 88.744(4)
_cell_angle_gamma                72.724(4)
_cell_formula_units_Z            2
_cell_length_a                   11.5671(14)
_cell_length_b                   13.5147(13)
_cell_length_c                   24.091(3)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    122.4
_cell_measurement_theta_max      29.845
_cell_measurement_theta_min      2.472
_cell_volume                     3487.5(7)
_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 0.998
_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  0.0990
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            110647
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.999
_diffrn_reflns_theta_min         2.352
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.7134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0815 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.9559.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'clear brownish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.321
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         22216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0280P)^2^+0.9710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14252
_reflns_number_total             22216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02077h2.cif
_cod_data_source_block           mo_d8v448_0m-1
_cod_depositor_comments
'Adding full bibliography for 1521279--1521290.cif.'
_cod_original_cell_volume        3487.6(7)
_cod_database_code               1521280
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.858
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C26(H26), C2(H2), C32(H32), C20(H20), C14(H14), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C19(H19A,H19B), C24(H24A,H24B), C3(H3A,H3B), C4(H4A,H4B),
 C37(H37A,H37B), C13(H13A,H13B), C34(H34A,H34B), C25(H25A,H25B), C12(H12A,H12B),
  C6(H6A,H6B), C33(H33A,H33B), C23(H23A,H23B), C29(H29A,H29B), C16(H16A,H16B),
 C15(H15A,H15B), C35(H35A,H35B), C27(H27A,H27B), C11(H11A,H11B), C17(H17A,H17B),
  C5(H5A,H5B), C21(H21A,H21B), C18(H18A,H18B), C7(H7A,H7B), C31(H31A,H31B),
 C10(H10A,H10B), C28(H28A,H28B), C9(H9A,H9B), C30(H30A,H30B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C72(H72), C63(H63), C49(H49), C61(H61), C67(H67), C43(H43), C64(H64),
 C69(H69), C47(H47), C45(H45), C70(H70), C40(H40), C66(H66), C55(H55), C59(H59),
  C73(H73), C57(H57), C60(H60), C71(H71), C48(H48), C42(H42), C51(H51),
 C41(H41), C39(H39), C46(H46), C58(H58), C54(H54), C53(H53), C65(H65), C52(H52)
;
_shelx_res_checksum              74203
_olex2_submission_special_instructions 'No special instructions were received'