Modular synthesis of pentaarylcyclopentadienyl Ru-based molecular machines via sequential Pd-catalysed cross couplings
Gisbert, Yohan; ABID, Seifallah; Bertrand, Gaelle; Kammerer, Claire; Rapenne, Gwenael; Saffon-Merceron, Nathalie; Chemical Communications  (2019) –; doi:10.1039/C9CC08384G

data_7124501
_publ_section_title
;
 Modular synthesis of pentaarylcyclopentadienyl Ru-based molecular
 machines via sequential Pd-catalysed cross couplings
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC08384G
_journal_year                    2019
_chemical_formula_sum            'C66.5 H57 B Br4 Cl3 I N6 Ru S3'
_chemical_formula_weight         1701.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-10-09 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.569(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1648(6)
_cell_length_b                   24.9566(10)
_cell_length_c                   21.5935(9)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.81
_cell_measurement_theta_min      2.78
_cell_volume                     6763.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8-Venture CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1196
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            118682
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.270
_diffrn_reflns_theta_max         67.270
_diffrn_reflns_theta_min         4.647
_diffrn_source                   'incoatec microfocus sealed tube'
_exptl_absorpt_coefficient_mu    10.534
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       plate
_exptl_crystal_F_000             3356
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.655
_refine_diff_density_min         -2.104
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         12080
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0737
_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^)+(0.0791P)^2^+72.8547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8648
_reflns_number_total             12080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08384g2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C66.50 H57 B Br4 Cl3 I N6 Ru S3'
_cod_database_code               7124501
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.227
_shelx_estimated_absorpt_t_max   0.678
_shelx_res_checksum              47501
_shelx_fab_checksum              1632