Solid and solution state flexibility of sterically congested bis(imino)bipyridine complexes of zinc(ii) and nickel(ii)
Griffith, Gerry A.; Al-Khatib, Mohamed J.; Patel, Kalpana; Singh, Kuldip; Solan, Gregory A.; Dalton Transactions  (2009) 185–196; doi:10.1039/b811309b

data_7000215
_publ_section_title
;
 Solid and solution state flexibility of sterically congested
 bis(imino)bipyridine complexes of zinc(ii) and nickel(ii)
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              185
_journal_page_last               196
_journal_paper_doi               10.1039/b811309b
_journal_year                    2009
_chemical_formula_moiety         ' C38 H46 Cl2 N4 Ni, 3(C H Cl3) '
_chemical_formula_sum            'C41 H49 Cl11 N4 Ni'
_chemical_formula_weight         1046.50
_chemical_name_systematic
;
?
;
_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                65.944(3)
_cell_angle_beta                 88.962(3)
_cell_angle_gamma                77.909(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8776(17)
_cell_length_b                   14.496(2)
_cell_length_c                   17.156(3)
_cell_measurement_reflns_used    837
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.176
_cell_measurement_theta_min      2.427
_cell_volume                     2408.6(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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  0.0779
_diffrn_reflns_av_sigmaI/netI    0.1612
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19018
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 6971 reflections(SADABS);Rint 0.0492 before
correction and 0.0293 after.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         9350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                4830
_reflns_number_total             9350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b811309b.txt
_cod_data_source_block           08018
_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:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        2408.6(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000215