Transition Metal Complexes of 3-Cyano- and 3-Nitroformazans
Joe B. Gilroy; Brian O. Patrick; Robert McDonald; Robin G. Hicks; Inorganic Chemistry 47 (2008) 1287–1294; doi:10.1021/ic7019846

data_4304485
_publ_section_title
;
Transition Metal Complexes of 3-Cyano- and 3-Nitroformazans
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1287
_journal_page_last               1294
_journal_paper_doi               10.1021/ic7019846
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C38 H46 N10 Ni2 O6, 0.5(C5 H12)'
_chemical_formula_sum            'C40.5 H52 N10 Ni2 O6'
_chemical_formula_weight         892.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 92.5918(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6602(14)
_cell_length_b                   19.801(2)
_cell_length_c                   19.807(2)
_cell_measurement_reflns_used    5571
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.24
_cell_volume                     4568.4(9)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19920
_diffrn_reflns_theta_full        27.66
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.8723
_exptl_absorpt_correction_T_min  0.6485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
 Attempts to refine peaks of residual electron density as solvent n-pentane
 carbon atoms were unsuccessful.  The data were corrected for disordered
 electron density through use of the SQUEEZE procedure (Sluis, P. van der;
 Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON
 (Spek, A. L. Acta Crystallogr. 1990, A46, C34.  PLATON - a multipurpose
 crystallographic tool.  Utrecht University, Utrecht, The Netherlands).
 A total solvent-accessible void volume of 647.9 A^3^ with a total electron
 count of 162 (consistent with two molecules of solvent n-pentane, or
 one-half molecule per formula unit of the nickel complex molecule) was
 found in the unit cell.
;
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0661P)^2^+1.5241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                4491
_reflns_number_total             5301
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic7019846-file002.cif
_cod_data_source_block           vic0714
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        4568.5(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C40.50 H52 N10 Ni2 O6'
_cod_database_code               4304485