Towards oxalate-bridged iron(ii), cobalt(ii), nickel(ii) and zinc(ii) complexes through oxotris(oxalato)niobate(v): an open air non-oxidizing synthetic route
Oliveira, Willian X. C.; Pereira, Cynthia L. M.; Pinheiro, Carlos B.; Lloret, Francesc; Julve, Miguel; Inorganic Chemistry Frontiers 5 (2018) 1294–; doi:10.1039/C8QI00191J

data_4349840
_publ_section_title
;
 Towards oxalate-bridged iron(ii), cobalt(ii), nickel(ii) and zinc(ii)
 complexes through oxotris(oxalato)niobate(v): an open air non-oxidizing
 synthetic route
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1294
_journal_paper_doi               10.1039/C8QI00191J
_journal_volume                  5
_journal_year                    2018
_chemical_formula_sum            'C62 H60 Cl2 Co2 N8 O14 S2'
_chemical_formula_weight         1394.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                82.207(8)
_cell_angle_beta                 84.709(8)
_cell_angle_gamma                71.837(9)
_cell_formula_units_Z            1
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_cell_length_b                   12.2165(12)
_cell_length_c                   13.0629(12)
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_cell_volume                     1550.1(3)
_computing_cell_refinement       'CysAlisPro 171.37.34b'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
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_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported S'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
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_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43439
_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         26.369
_diffrn_reflns_theta_min         2.282
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Thu Jun 18 12:11:23 2015'
;
_exptl_crystal_colour            Plate
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_meas      Pink
_exptl_crystal_description
;
'Thu Jun 18 12:11:23 2015'
;
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.200
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_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.071
_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     422
_refine_ls_number_reflns         6331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+1.3647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4523
_reflns_number_total             6331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00191j2.cif
_cod_data_source_block           shelx_CCDC2
_cod_database_code               4349840
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.863
_shelx_estimated_absorpt_t_max   0.942
_shelx_res_checksum              4865
_shelx_hkl_checksum              83483