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_7123047
_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 H88 Au4 Cu2 N4 O12 P4 Pd2 S4, 4(N O3), 4(H2 O)'
_chemical_formula_sum            'C70 H96 Au4 Cu2 N8 O28 P4 Pd2 S4'
_chemical_formula_weight         2877.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8393(17)
_cell_length_b                   20.715(2)
_cell_length_c                   26.283(3)
_cell_measurement_reflns_used    15560
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      1.19
_cell_volume                     9168.2(17)
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_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 14.69
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury2CCD detector'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  Si(311)
_diffrn_radiation_source         'SPring-8 BL02B1 bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7002
_diffrn_reflns_av_R_equivalents  0.1746
_diffrn_reflns_av_unetI/netI     0.2300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            45169
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.842
_diffrn_reflns_theta_max         27.044
_diffrn_reflns_theta_min         1.233
_exptl_absorpt_coefficient_mu    7.126
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2464
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_description       block
_exptl_crystal_F_000             5544
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.526
_refine_diff_density_min         -3.810
_refine_diff_density_rms         0.301
_refine_ls_abs_structure_details
;
 Flack x determined using 2857 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1107
_refine_ls_number_reflns         20968
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1742
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                12014
_reflns_number_total             20968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00152b2.cif
_cod_data_source_block           '[2](NO3)4'
_cod_original_cell_volume        9167.9(17)
_cod_database_code               7123047
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.536
_shelx_estimated_absorpt_t_max   0.536
_shelx_res_checksum              89157