Bis(2,2'-bipyridine)bis{μ~3~-<i>cis</i>-<i>N</i>-(2-carboxylatophenyl)-<i>N</i>'-[3-(dimethylamino)propyl]oxamidato(3{-})}bis(perchlorato)tetranickel(II) methanol disolvate
Tian, Chunliang; Gao, Zhongjun; Acta Crystallographica Section E 65 (2009) m1691–; doi:10.1107/S160053680905017X

data_2224405
_publ_section_title
;Bis(2,2'-bipyridine)bis{\m~3~-<i>cis</i>-<i>N</i>-(2-carboxylatophenyl)-<i>N</i>'-[3-(dimethylamino)propyl]oxamidato(3{-})}bis(perchlorato)tetranickel(II)
 methanol disolvate
;
_journal_coeditor_code           PV2236
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1691
_journal_paper_doi               10.1107/S160053680905017X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni4 (C14 H16 N3 O4)2 (Cl O4)2 (C10 H8 N2)2]'
_chemical_formula_moiety         'C48 H48 Cl2 N10 Ni4 O16, 2(C H4 O)'
_chemical_formula_sum            'C50 H56 Cl2 N10 Ni4 O18'
_chemical_formula_weight         1390.79
_chemical_name_systematic
;Bis(2,2'-bipyridine)bis{\m~3~-<i>cis</i>-<i>N</i>-(2-carboxylatophenyl)-
<i>N</i>'-[3-(dimethylamino)propyl]oxamidato(3-)}bis(perchlorato)tetranickel(II)
methanol
 disolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.724(4)
_cell_angle_beta                 73.357(4)
_cell_angle_gamma                75.411(4)
_cell_formula_units_Z            1
_cell_length_a                   10.854(4)
_cell_length_b                   11.309(4)
_cell_length_c                   12.728(5)
_cell_measurement_reflns_used    3928
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.142
_cell_measurement_theta_min      2.175
_cell_volume                     1367.0(9)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\f and \w 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  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7296
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  0.8135
_exptl_absorpt_correction_T_min  0.7383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.556
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.6427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                3963
_reflns_number_total             4850
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pv2236.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2224405
_cod_database_fobs_code          2224405