Synthesis, crystal structures and magneto-structural correlations study of three 3d metal-radical heterospin complexes
Yuan-Yuan Gao; Ming-Fang Yang; Ning Han, Yue Ma; Ya-Li Wang; Yu-Zhang Tong; Qing-Lun Wang; Li-Cun Li; Dai-Zheng Liao; Inorganica Chimica Acta 397 (2013) 32–37; doi:10.1016/j.ica.2012.11.013

data_1513017
_publ_section_title
;
 Synthesis, crystal structures and magneto-structural correlations study
 of three 3d metal-radical heterospin complexes
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              32
_journal_page_last               37
_journal_paper_doi               10.1016/j.ica.2012.11.013
_journal_volume                  397
_journal_year                    2013
_chemical_formula_sum            'C31 H37 Cu N7 O10'
_chemical_formula_weight         731.22
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2675(19)
_cell_length_b                   10.2369(14)
_cell_length_c                   24.371(4)
_cell_measurement_reflns_used    5560
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.05
_cell_measurement_theta_min      2.16
_cell_volume                     3310.0(9)
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16926
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         5618
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+2.3767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1283
_reflns_number_gt                5117
_reflns_number_total             5618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-397-32-37-1.cif
_cod_data_source_block           51128d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3310.0(8)
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               1513017