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_4088008
_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         'C40 H66 N4 P2 Ru, 2(C24 H20 P), 6(C H Cl3)'
_chemical_formula_sum            'C94 H112 Cl18 N4 P4 Ru'
_chemical_formula_weight         2161.07
_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_Int_Tables_number      2
_audit_creation_date             2015-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                88.966(15)
_cell_angle_beta                 76.208(15)
_cell_angle_gamma                67.398(14)
_cell_formula_units_Z            1
_cell_length_a                   12.421(4)
_cell_length_b                   13.919(4)
_cell_length_c                   16.511(6)
_cell_measurement_reflns_used    8717
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      2.48
_cell_volume                     2550.7(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            110335
_diffrn_reflns_theta_full        27.1024
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         12.10
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1309 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.8350.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.4067
_exptl_crystal_description       prism
_exptl_crystal_F_000             1116.1147
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.171
_refine_diff_density_max         1.3511
_refine_diff_density_min         -1.1806
_refine_diff_density_rms         0.1124
_refine_ls_d_res_high            0.7800
_refine_ls_d_res_low             9.7144
_refine_ls_goodness_of_fit_ref   1.0683
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    106
_refine_ls_number_parameters     630
_refine_ls_number_reflns         11246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0683
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.0070
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0841P)^2^+6.7922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.1826
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                9443
_reflns_number_total             11246
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            Ru(CN)4(PCy3)2.cif
_cod_data_source_block           mo_d8v1244_0m-good
_cod_original_cell_volume        2550.8(15)
_cod_database_code               4088008
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Sof(H6b)=Sof(Cl2A)=Sof(Cl6A)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(Cl6)=Sof(H6a)=FVAR(1)
 Sof(H10a)=Sof(Cl5A)=Sof(Cl3A)=Sof(Cl8A)=1-FVAR(2)
 Sof(Cl3)=Sof(Cl5)=Sof(Cl8)=Sof(H10)=FVAR(2)
 Sof(H65a)=Sof(Cl9A)=Sof(Cl7A)=Sof(Cl4A)=1-FVAR(3)
 Sof(H65)=Sof(Cl4)=Sof(Cl7)=Sof(Cl9)=FVAR(3)
3.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C33(H33), C65(H65), C65(H65a), C6(H6b), C6(H6a),
 C10(H10a), C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C13(H13a,H13b), C15(H15a,H15b), C16(H16a,H16b), C18(H18a,H18b),
 C21(H21a,H21b), C27(H27a,H27b), C29(H29a,H29b), C30(H30a,H30b), C32(H32a,H32b),
  C38(H38a,H38b), C41(H41a,H41b), C46(H46a,H46b), C49(H49a,H49b), C50(H50a,H50b)
3.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C24(H24), C25(H25), C26(H26), C28(H28), C35(H35), C36(H36),
 C42(H42), C45(H45), C47(H47), C48(H48), C51(H51), C55(H55), C56(H56), C57(H57),
  C59(H59), C60(H60), C62(H62), C63(H63), C64(H64)
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_olex2_submission_special_instructions 'No special instructions were received'