Phosphine Substitution and Linkage Isomerization in Cyclopentadienylruthenium bis(triphenylphosphine)thiocyanide and selenocyanide, CpRu(PPh3)2NCS and CpRu(PPh3)2SeCN
Dang, Duy-Khoi; Cehreli, Damla; Rich, Benjamin S.; Haas, Terry E.; Fronczek, Frank R.; Kirss, Rein; Dalton Transactions  (2023) –; doi:10.1039/D3DT02397D

data_7713846
_publ_section_title
;
 Phosphine Substitution and Linkage Isomerization in
 Cyclopentadienylruthenium bis(triphenylphosphine)thiocyanide and
 selenocyanide, CpRu(PPh3)2NCS and CpRu(PPh3)2SeCN
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02397D
_journal_year                    2023
_chemical_formula_sum            'C43 H37 Cl2 N P2 Ru S'
_chemical_formula_weight         833.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-18 deposited with the CCDC.	2023-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3288(10)
_cell_length_b                   20.6729(10)
_cell_length_c                   8.8263(4)
_cell_measurement_reflns_used    9555
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.4608
_cell_measurement_theta_min      2.5092
_cell_volume                     3709.3(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'Photon II area detector'
_diffrn_measurement_method       'generic \w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            147851
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.405
_diffrn_reflns_theta_min         2.811
_diffrn_source                   'Mo fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.7411
_exptl_absorpt_correction_T_min  0.698880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2  Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            'intense yellow'
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 2839 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(10)
_refine_ls_extinction_coef       0.00072(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6820
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0067P)^2^+10.1039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6296
_reflns_number_total             6820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02397d2.cif
_cod_data_source_block           1a
_cod_database_code               7713846
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              3423