Anion exchange coupled with the reduction and dimerisation of a copper(ii) nitrate complex of tripyridyl dithioether via a single-crystal-to-single-crystal transformation
Lee, Hyeong-Hwan; Park, In-Hyeok; Kim, Seulgi; Lee, Eunji; Ju, Huiyeong; Jung, Jong Hwa; Ikeda, Mari; Habata, Yoichi; Lee, Shim Sung; Chem. Sci. 8 (2017) 2592–; doi:10.1039/C6SC05341F

data_1544984
_publ_section_title
;
 Anion exchange coupled with the reduction and dimerisation of a
 copper(ii) nitrate complex of tripyridyl dithioether via a
 single-crystal-to-single-crystal transformation
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2592
_journal_paper_doi               10.1039/C6SC05341F
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C34 H30 Cu4 I4 N6 S4'
_chemical_formula_weight         1412.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-31 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                101.5230(10)
_cell_angle_beta                 102.9950(10)
_cell_angle_gamma                104.2830(10)
_cell_formula_units_Z            1
_cell_length_a                   8.81100(10)
_cell_length_b                   10.09970(10)
_cell_length_c                   12.5440(2)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.49
_cell_volume                     1014.82(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0224
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16176
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.730
_exptl_absorpt_coefficient_mu    5.350
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.311
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_exptl_transmission_factor_max   0.5910
_exptl_transmission_factor_min   0.2710
_refine_diff_density_max         0.655
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+0.5021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3791
_reflns_number_total             3994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc05341f2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 1544983--1544989.cif.'
_cod_database_code               1544984
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.271
_shelx_estimated_absorpt_t_max   0.591
_shelx_res_checksum              74123
_shelx_hkl_checksum              66870