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_4349841
_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            'C186 H144 N24 Nb2 Ni6 O52.19'
_chemical_formula_weight         4088.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.7961(16)
_cell_length_b                   33.5952(13)
_cell_length_c                   33.0784(18)
_cell_measurement_reflns_used    22433
_cell_measurement_temperature    150(2)
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_cell_measurement_theta_min      2.4820
_cell_volume                     39779(3)
_computing_cell_refinement       'CysAlisPro 171.37.34b'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'CysAlisPro 171.37.34b'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
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'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  0.0613
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            121551
_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         26.372
_diffrn_reflns_theta_min         1.676
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Tue Mar 31 18:37:32 2015'
;
_exptl_crystal_colour            'Light Blue'
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       Block
_exptl_crystal_F_000             16764
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.729
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.427(17)
_refine_ls_extinction_coef       0.000116(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         19513
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0640
_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^)+(0.1213P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                15692
_reflns_number_total             19513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00191j2.cif
_cod_data_source_block           shelx_CCDC3
_cod_database_code               4349841
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              56565
_shelx_hkl_checksum              49073