Carbocyclic pincer carbene complexes of ruthenium: syntheses and reversible hydrogenation.
Wiedmaier, Nicholas R.; Schubert, Hartmut; Mayer, Hermann A.; Wesemann, Lars; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11814–11820; doi:10.1039/d1dt02266k

data_7707982
_publ_section_title
;
 Carbocyclic pincer carbene complexes of ruthenium: syntheses and
 reversible hydrogenation.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11814
_journal_page_last               11820
_journal_paper_doi               10.1039/d1dt02266k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'C31.33333 H48.66667 Cl2 P2 Ru'
_chemical_formula_weight         659.28
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2020-10-14 deposited with the CCDC.	2021-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                67.4590(10)
_cell_angle_beta                 89.6070(10)
_cell_angle_gamma                88.4290(10)
_cell_formula_units_Z            3
_cell_length_a                   12.1104(2)
_cell_length_b                   14.1717(3)
_cell_length_c                   14.9865(3)
_cell_measurement_reflns_used    9292
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.94
_cell_volume                     2374.65(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            69257
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         3.731
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       prism
_exptl_crystal_F_000             1034
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.331
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 8983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         20132
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0361P)^2^+0.8728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.939
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                19390
_reflns_number_total             20132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02266k2.cif
_cod_data_source_block           NW105_0m
_cod_depositor_comments
;
Adding full bibliography for 7707980--7707982.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C94 H146 Cl6 P6 Ru3'
_cod_original_formula_weight         1977.83
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2374.66(8)
_cod_database_code               7707982
_shelxl_version_number           2014-3
_shelx_res_checksum              54203
_shelx_hkl_checksum              7049