Ligand Sphere Conversions in Terminal Carbide Complexes
Morsing, Thorbjørn J.; Reinholdt, Anders; Sauer, Stephan P. A.; Bendix, Jesper; Organometallics 35 (2015) 100–; doi:10.1021/acs.organomet.5b00803

data_4088013
_publ_section_title
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 Ligand Sphere Conversions in Terminal Carbide Complexes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              100
_journal_paper_doi               10.1021/acs.organomet.5b00803
_journal_volume                  35
_journal_year                    2015
_chemical_formula_moiety         'C39 H69 Cl N P2 Ru, C F3 O3 S'
_chemical_formula_sum            'C40 H69 Cl F3 N O3 P2 Ru S'
_chemical_formula_weight         899.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                81.185(6)
_cell_angle_beta                 86.493(6)
_cell_angle_gamma                72.928(6)
_cell_formula_units_Z            2
_cell_length_a                   10.0150(16)
_cell_length_b                   14.317(2)
_cell_length_c                   15.830(2)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.22
_cell_volume                     2143.8(5)
_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 0.999
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            106298
_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         27.103
_diffrn_reflns_theta_min         2.223
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1399 before and 0.0809 after correction.
The Ratio of minimum to maximum transmission is 0.9370.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       prism
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         9456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0248P)^2^+2.0887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8548
_reflns_number_total             9456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            RuC-NCCH3.cif
_cod_data_source_block           mo_d8v1156_0m
_cod_original_cell_volume        2143.9(6)
_cod_database_code               4088013
_shelxl_version_number           2013-3
_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.a Ternary CH refined with riding coordinates:
 C4(H4), C16(H16), C10(H10), C34(H34), C22(H22), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C21(H21A,
 H21B), C20(H20A,H20B), C19(H19A,H19B), C18(H18A,H18B), C17(H17A,H17B),
 C15(H15A,H15B), C14(H14A,H14B), C13(H13A,H13B), C12(H12A,H12B), C11(H11A,H11B),
  C39(H39A,H39B), C38(H38A,H38B), C37(H37A,H37B), C36(H36A,H36B), C35(H35A,
 H35B), C27(H27A,H27B), C26(H26A,H26B), C25(H25A,H25B), C24(H24A,H24B),
 C23(H23A,H23B), C33(H33A,H33B), C32(H32A,H32B), C31(H31A,H31B), C30(H30A,H30B),
  C29(H29A,H29B)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
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_shelx_res_checksum              36026
_shelx_hkl_checksum              38412
_olex2_submission_special_instructions 'No special instructions were received'