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_7123046
_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
'C70 H84 Au4 Cu2 N4 O10 P4 Pd2 S4, 4(N O3), 3(H2 O)'
_chemical_formula_sum            'C70 H90 Au4 Cu2 N8 O25 P4 Pd2 S4'
_chemical_formula_weight         2823.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-14 deposited with the CCDC.    2019-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.43(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.842(4)
_cell_length_b                   17.342(4)
_cell_length_c                   25.184(5)
_cell_measurement_reflns_used    108842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.886
_cell_measurement_theta_min      1.443
_cell_volume                     9045(3)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    Mercury
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 210mm
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'ADSC Quantum210'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.630
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_unetI/netI     0.1799
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            64252
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         29.886
_diffrn_reflns_theta_min         1.443
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    5.490
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_description       block
_exptl_crystal_F_000             5424
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.046
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.026
_refine_diff_density_max         3.698
_refine_diff_density_min         -3.860
_refine_diff_density_rms         0.253
_refine_ls_abs_structure_details
;
 Flack x determined using 5562 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         35656
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0523P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1536
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                17256
_reflns_number_total             35656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00152b2.cif
_cod_data_source_block           '[3](NO3)4'
_cod_database_code               7123046
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              62522