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_4088010
_publ_section_title
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 Ligand Sphere Conversions in Terminal Carbide Complexes
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_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         'C38 H66 Cl N O P2 Ru'
_chemical_formula_sum            'C38 H66 Cl N O P2 Ru'
_chemical_formula_weight         751.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 115.4970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1947(4)
_cell_length_b                   23.4389(7)
_cell_length_c                   13.5623(4)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      30.24
_cell_measurement_theta_min      2.41
_cell_volume                     3785.9(2)
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            55196
_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         25.681
_diffrn_reflns_theta_min         2.406
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1088 before and 0.0565 after correction.
The Ratio of minimum to maximum transmission is 0.9450.
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    1.318
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7186
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0251P)^2^+3.7419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6244
_reflns_number_total             7186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            RuC-NCO.cif
_cod_data_source_block           mo_d8v266_0m-ny
_cod_database_code               4088010
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.882
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C34A-H34D = C34A-H34C
 0.99 with sigma of 0.001
 H28B-H34D
 2.05 with sigma of 0.001
 Ru1-Cl1A \\sim Ru1-Cl1
 with sigma of 0.001
 Ru1-N1A \\sim Ru1-N1
 with sigma of 0.001
 N1-C2 \\sim N1A-C2A
 with sigma of 0.001
 O1A-C2A \\sim O1-C2
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uiso(C2A) = Uiso(N1A)
4. Others
 Sof(Cl1A)=Sof(N1A)=Sof(C2A)=Sof(O1A)=1-FVAR(1)
 Sof(Cl1)=Sof(N1)=Sof(O1)=Sof(C2)=FVAR(1)
 Sof(H33A)=Sof(H36C)=Sof(H36D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C34A)=
 Sof(H34C)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=
 Sof(H34D)=1-FVAR(2)
 Sof(H33)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H36A)=Sof(H36B)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C34)=Sof(H34A)=Sof(H34B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C27(H27), C33(H33), C33(H33A), C3(H3), C9(H9), C15(H15), C21(H21)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C19(H19A,H19B), C14(H14A,H14B), C17(H17A,H17B), C16(H16A,
 H16B), C32(H32A,H32B), C20(H20A,H20B), C22(H22A,H22B), C28(H28A,H28B),
 C29(H29A,H29B), C8(H8A,H8B), C13(H13A,H13B), C18(H18A,H18B), C7(H7A,H7B),
 C26(H26A,H26B), C11(H11A,H11B), C38(H38A,H38B), C23(H23A,H23B), C31(H31A,H31B),
  C30(H30A,H30B), C36(H36A,H36B), C36(H36C,H36D), C25(H25B,H25A), C4(H4A,H4B),
 C35(H35A,H35B), C6(H6A,H6B), C24(H24A,H24B), C5(H5A,H5B), C12(H12A,H12B),
 C37(H37A,H37B), C34(H34A,H34B), C35A(H35C,H35D), C37A(H37C,H37D), C38A(H38C,
 H38D)
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_shelx_res_checksum              29813
_shelx_hkl_checksum              66988
_olex2_submission_special_instructions 'No special instructions were received'