Crystal-to-crystal interconversion of open and closed dicopper(II) paddle-wheels in a heterotrimetallic coordination polymer
Ohwaki, Hayato; Yoshinari, Nobuto; Konno, Takumi; Chemical Communications  (2019) –; doi:10.1039/C9CC00152B

data_7123045
_publ_section_title
;
 Crystal-to-crystal interconversion of open and closed dicopper(II)
 paddle-wheels in a heterotrimetallic coordination polymer
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00152B
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_moiety
'4(C35 H40 Au2 N2 O4 P2 Pd S2), C2 H5 O, 46(O)'
_chemical_formula_sum            'C142 H258 Au8 N8 O63 P8 Pd4 S8'
_chemical_formula_weight         5591.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-27 deposited with the CCDC.    2019-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.887(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.2767(3)
_cell_length_b                   37.3828(7)
_cell_length_c                   16.9637(3)
_cell_measurement_reflns_used    35497
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      32.78
_cell_measurement_theta_min      3.00
_cell_volume                     10168.6(4)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'Mercury 3.10'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku R-AXIS VII'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.1155
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58147
_diffrn_reflns_point_group_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.001
_diffrn_source                   'Rigaku FR-E SuperBright'
_exptl_absorpt_coefficient_mu    6.313
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_correction_T_min  0.5551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_description       block
_exptl_crystal_F_000             5468
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_refine_diff_density_max         2.254
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details
;
 Flack x determined using 10088 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.051(4)
_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     2181
_refine_ls_number_reflns         40700
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0349P)^2^+25.9847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.788
_reflns_Friedel_fraction_full    0.814
_reflns_Friedel_fraction_max     0.782
_reflns_number_gt                31978
_reflns_number_total             40700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00152b2.cif
_cod_data_source_block           '[1]'
_cod_database_code               7123045
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.571
_shelx_estimated_absorpt_t_max   0.571
_shelx_res_checksum              31054