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_7223883
_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            'C296 H264 B11 Co4 F80 N80 Na O16 P6 Ru4'
_chemical_formula_weight         7685.58
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_symmetry_space_group_name_Hall  'P -4 2ab'
_symmetry_space_group_name_H-M   'P -4 21 m'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   31.3553(12)
_cell_length_b                   31.3553(12)
_cell_length_c                   21.7210(8)
_cell_measurement_reflns_used    9250
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.69
_cell_measurement_theta_min      2.26
_cell_volume                     21355.1(14)
_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_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0648
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_laue_measured_fraction_full 0.964
_diffrn_reflns_laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51397
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        23.499
_diffrn_reflns_theta_max         23.499
_diffrn_reflns_theta_min         0.918
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       cube
_exptl_crystal_F_000             7776
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3NO2, THF'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         15202
_refine_ls_number_restraints     832
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0794
_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^)+(0.1603P)^2^+25.9254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.2499
_reflns_Friedel_coverage         0.868
_reflns_friedel_fraction_full    0.966
_reflns_friedel_fraction_max     0.966
_reflns_number_gt                10893
_reflns_number_total             15202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra22694e2.cif
_cod_data_source_block           p421m_sq
_cod_original_cell_volume        21355.1(18)
_cod_database_code               7223883
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              62159
_shelx_fab_checksum              59105