Stepwise synthesis of mixed-metal assemblies using pre-formed Ru(II) ‘complex ligands’ as building blocks
Metherell, Alexander; Ward, Michael D.; RSC Adv.  (2016) –; doi:10.1039/C5RA22694E

data_7223885
_publ_section_title
;
 Stepwise synthesis of mixed-metal assemblies using pre-formed Ru(II)
 &#x2018;complex ligands&#x2019; as building blocks
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA22694E
_journal_year                    2016
_chemical_formula_sum            'C274 H235 B10 Co4 F76 N77 O2 P6 Ru4 S12'
_chemical_formula_weight         7401.02
_chemical_properties_physical    Efflorescent
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-01-06 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1010(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.3091(12)
_cell_length_b                   42.874(3)
_cell_length_c                   22.2336(16)
_cell_measurement_reflns_used    84009
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      1.3
_cell_volume                     16070(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.2356
_diffrn_reflns_av_unetI/netI     0.1313
_diffrn_reflns_laue_measured_fraction_full 0.973
_diffrn_reflns_laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74949
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        20.500
_diffrn_reflns_theta_max         20.500
_diffrn_reflns_theta_min         1.296
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DTABSCOR
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       Needle
_exptl_crystal_F_000             7468
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN, diethyl ether'
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1901
_refine_ls_number_reflns         17217
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1731
_refine_ls_R_factor_gt           0.1088
_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^)+(0.1894P)^2^+106.1160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2800
_refine_ls_wR_factor_ref         0.3405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9860
_reflns_number_total             17217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra22694e2.cif
_cod_data_source_block           p21c_sq
_cod_database_code               7223885
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              30966
_shelx_fab_checksum              1882