Novel tandem synthesis of bis(μ-NN'-tetrazolate) bridged dinuclear nickel(ii) Schiff base complex via [3 + 2] cyclo-addition at ambient condition.
Das, Mithun; Harms, Klaus; Chattopadhyay, Shouvik; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5643–5647; doi:10.1039/c3dt52398e

data_7029452
_publ_section_title
;
 Novel tandem synthesis of bis(\m-NN'-tetrazolate) bridged dinuclear
 nickel(ii) Schiff base complex via [3 + 2] cyclo-addition at ambient
 condition.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5643
_journal_page_last               5647
_journal_paper_doi               10.1039/c3dt52398e
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C34 H40 N16 Ni2 O4, 2(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C38 H50 N18 Ni2 O6'
_chemical_formula_weight         972.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.1600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3833(8)
_cell_length_b                   9.8759(6)
_cell_length_c                   17.7659(11)
_cell_measurement_reflns_used    7920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.44
_cell_volume                     2204.3(2)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER APEX II'
_computing_data_reduction        'Bruker APEX II'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25325
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         2.422
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6994
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       nugget
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+2.2096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4049
_reflns_number_total             5029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52398e.txt
_cod_data_source_block           s29_0m
_cod_database_code               7029452
_shelx_estimated_absorpt_t_min   0.816
_shelx_estimated_absorpt_t_max   0.859
_shelxl_version_number           2013-4
_shelx_res_checksum              95050
_shelx_hkl_checksum              1011