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_4088011
_publ_section_title
;
 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         'C37 H66 Br Cl P2 Ru'
_chemical_formula_sum            'C37 H66 Br Cl P2 Ru'
_chemical_formula_weight         789.26
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.7250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2074(5)
_cell_length_b                   23.3788(9)
_cell_length_c                   13.6727(5)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      27.494
_cell_measurement_theta_min      2.402
_cell_volume                     3803.3(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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  0.0571
_diffrn_reflns_av_unetI/netI     0.0303
_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       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58146
_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         26.732
_diffrn_reflns_theta_min         2.402
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.641
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0676 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.9104.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         8071
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0180P)^2^+3.0700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6798
_reflns_number_total             8071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            RuC-Br.cif
_cod_data_source_block           mo_d8v1210_0m-1
_cod_original_cell_volume        3803.3(2)
_cod_database_code               4088011
_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
2. Restrained distances
 Ru1-Br1 \\sim Ru1-Br1A
 with sigma of 0.001
 Ru1-Cl1A \\sim Ru1-Cl1
 with sigma of 0.001
3. Others
 Sof(Br1)=Sof(Cl1)=1-FVAR(1)
 Sof(Cl1A)=Sof(Br1A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C20(H20), C14(H14), C2(H2), C32(H32), C26(H26), C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C30(H30A,H30B), C22(H22A,H22B), C11(H11A,H11B), C31(H31A,
 H31B), C29(H29A,H29B), C33(H33A,H33B), C7(H7A,H7B), C28(H28A,H28B), C27(H27A,
 H27B), C13(H13A,H13B), C34(H34A,H34B), C23(H23A,H23B), C9(H9A,H9B), C10(H10A,
 H10B), C25(H25A,H25B), C37(H37A,H37B), C19(H19A,H19B), C18(H18A,H18B),
 C36(H36A,H36B), C6(H6A,H6B), C16(H16A,H16B), C17(H17A,H17B), C15(H15A,H15B),
 C4(H4A,H4B), C35(H35A,H35B), C5(H5A,H5B), C12(H12A,H12B), C24(H24A,H24B),
 C3(H3A,H3B)
;
_shelx_res_checksum              80876
_shelx_hkl_checksum              80803
_olex2_submission_special_instructions 'No special instructions were received'