Formation of bis(μ-tetrazolato)dinickel(ii) complexes with N,N,O-donor Schiff bases via in situ 1,3-dipolar cyclo-additions: isolation of a novel bi-cyclic trinuclear nickel(ii)-sodium(i)-nickel(ii) complex.
Das, Mithun; Chatterjee, Sudipta; Harms, Klaus; Mondal, Tapan Kumar; Chattopadhyay, Shouvik; Dalton transactions (Cambridge, England : 2003) 43 (2014) 2936–2947; doi:10.1039/c3dt52796d

data_7028467
_publ_section_title
;
 Formation of bis(\m-tetrazolato)dinickel(ii) complexes with N,N,O-donor
 Schiff bases via in situ 1,3-dipolar cyclo-additions: isolation of a
 novel bi-cyclic trinuclear nickel(ii)-sodium(i)-nickel(ii) complex.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2936
_journal_page_last               2947
_journal_paper_doi               10.1039/c3dt52796d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C34 H40 N14 Na Ni2 O5, Cl O4, H2 O'
_chemical_formula_sum            'C34 H40 Cl N14 Na Ni2 O9'
_chemical_formula_weight         982.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.7190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8601(3)
_cell_length_b                   20.9255(5)
_cell_length_c                   22.4384(6)
_cell_measurement_reflns_used    66876
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.7
_cell_measurement_theta_min      1.8
_cell_volume                     5073.8(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX V1.80.05'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  '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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66876
_diffrn_reflns_theta_full        24.67
_diffrn_reflns_theta_max         24.67
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_correction_T_min  0.8889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(R.H. Blessing, Acta Crystallogr., Sect A 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             1865
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
SQUEEZE was used to remove the contributions of one solvent water molecule.
;
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         8522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                5871
_reflns_number_total             8522
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt52796d.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-Scan'
changed to 'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7028467
_alert_response
;
Alert C CHEMW01, CHEMW03, DENSD01, PLAT046, PLAT068 Calculated and 
Reported Values for formula, absorption coefficient, molecular mass and F000 value.
Response
One water molecule was present as the solvent molecule which was 
removed using SQUEEZE. Thus two hydrogen atoms and one oxygen atom 
of water molecule were added to the chemical formula to adjust 
the density, molecular mass and F000 value. 
Results in the chemical_formula_moiety 
C34 H40 N14 Na Ni2 O5, Cl O4, H2 O.

;