Croconato-bridged copper(II) complexes. Synthesis, structure and magnetic characterization
Massoud, Salah S.; Williams, Gabrielle F.; Louka, Febee R.; Henary, Maher M.; Herchel, Radovan; Travnicek, Zdenek; Fischer, Roland; Mautner, Franz Andreas; New J. Chem. 41 (2017) 3846–3856; doi:10.1039/C6NJ03943J

data_7056086
_publ_section_title
;
 Croconato-bridged copper(II) complexes. Synthesis, structure and magnetic
 characterization
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              3846
_journal_page_last               3856
_journal_paper_doi               10.1039/C6NJ03943J
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C45 H44 Cu2 N8 O5, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C45 H48 Cl2 Cu2 N8 O15'
_chemical_formula_weight         1138.91
_chemical_name_common            '[Cu2(C5O5)(pmap)2](ClO4)2.2H2O'
_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   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-03-30 deposited with the CCDC.
2017-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.511(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6600(12)
_cell_length_b                   16.0434(13)
_cell_length_c                   20.4427(18)
_cell_measurement_reflns_used    4000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.50
_cell_volume                     4810.4(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            82504
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.388
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  0.9384
_exptl_absorpt_correction_T_min  0.7117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       prism
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.060
_exptl_transmission_factor_max   0.938
_exptl_transmission_factor_min   0.712
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1493
_refine_ls_number_reflns         17785
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+22.9440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                13819
_reflns_number_total             17785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03943j2.cif
_cod_data_source_block           rf1150s
_cod_database_code               7056086
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.712
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              41278