Synthesis, crystal structure, magnetic and electrochemical studies of two copper complexes with carboxylate rich dinucleating ligand
Rebecca A. Joy; Hadi Arman; Shengchang Xiang; Ghezai T. Musie; Inorganica Chimica Acta 393 (2012) 220–228; doi:

data_1512732
_publ_section_title
;
 Synthesis, crystal structure, magnetic and electrochemical studies of two
 copper complexes with carboxylate rich dinucleating ligand
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              220
_journal_page_last               228
_journal_volume                  393
_journal_year                    2012
_chemical_formula_moiety
'2(C24 H31 Cu2 K3 N2 O17), 2(C3 H6 O), 3.5(H2 O)'
_chemical_formula_sum            'C54 H81 Cu4 K6 N4 O39.5'
_chemical_formula_weight         1907.03
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                97.910(6)
_cell_angle_beta                 100.740(7)
_cell_angle_gamma                109.900(7)
_cell_formula_units_Z            1
_cell_length_a                   9.4973(8)
_cell_length_b                   11.6634(11)
_cell_length_c                   18.2100(17)
_cell_measurement_reflns_used    8727
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      2.0
_cell_volume                     1818.8(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14348
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.597
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             979
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.0087(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+3.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                7985
_reflns_number_total             8226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-220-228-1.cif
_cod_data_source_block           K3Cu2ccdp
_cod_original_formula_sum        'C54 H81 Cu4 K6 N4 O39.50'
_cod_database_code               1512732