C,Cʹ-Ru to C,Bʹ-Ru Isomerisation in Bis(phosphine)Ru Complexes of [1,1ʹ-Bis(ortho-carborane)]
Jeans, Rebekah; Rosair, Georgina; Welch, Alan Jeffrey; Chemical Communications  (2021) –; doi:10.1039/D1CC06119D

data_7129335
_publ_section_title
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 C,C&#x02B9;-Ru to C,B&#x02B9;-Ru Isomerisation in Bis(phosphine)Ru
 Complexes of [1,1&#x02B9;-Bis(ortho-carborane)]
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06119D
_journal_year                    2021
_chemical_formula_moiety         'C30 H46 B20 P2 Ru, C0.5 H Cl0.998'
_chemical_formula_sum            'C30.5 H47 B20 Cl P2 Ru'
_chemical_formula_weight         828.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-23 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.8580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.0931(9)
_cell_length_b                   10.6717(3)
_cell_length_c                   21.3413(5)
_cell_measurement_reflns_used    9276
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.60
_cell_measurement_theta_min      3.92
_cell_volume                     8051.9(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            64154
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.729
_diffrn_reflns_theta_min         2.499
_exptl_absorpt_coefficient_mu    4.678
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0881 before and 0.0457 after correction. The Ratio of minimum to maximum transmission is 0.7192. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             3367
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8221
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+12.1039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8203
_reflns_number_total             8221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06119d2.cif
_cod_data_source_block           8v00099_0m
_cod_original_formula_sum        'C30.50 H47 B20 Cl P2 Ru'
_cod_database_code               7129335
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.455
_shelx_estimated_absorpt_t_min   0.269
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-C1S \\sim Cl2-C1S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Others
 1*[Sof(Cl1)]+1*[Sof(Cl2)]+1*[Sof(Cl1A)]=1 with esd of 0.01
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C202(H202), C203(H203),
 C204(H204), C205(H205), C206(H206), C211(H211), C212(H212), C213(H213),
 C214(H214), C215(H215)
5.b Idealised Me refined as rotating group:
 C100(H10A,H10B,H10C), C200(H20A,H20B,H20C)
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_shelx_res_checksum              34527
_olex2_submission_special_instructions 'No special instructions were received'