Synthesis, structure and characterization of novel nickel(II) and iron(II) complexes with a 5,5′-bis[2-(2,2′-bipyridin-6-yl)-ethyl]-2,2′-bipyridine ligand
Shu, Mou-Hai; Duan, Chun-Ying; Sun, Wei-Yin; Fu, You-Jun; Zhang, Dao-Hua; Bai, Zhi-Ping; Tang, Wen-Xia; Journal of the Chemical Society, Dalton Transactions  (1999) 2317–; doi:10.1039/a901835b

data_7027361
_publ_section_title
;
 Synthesis, structure and characterization of novel nickel(II) and
 iron(II) complexes with a
 5,5&#x2032;-bis[2-(2,2&#x2032;-bipyridin-6-yl)-ethyl]-2,2&#x2032;-bipyridine
 ligand
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2317
_journal_paper_doi               10.1039/a901835b
_journal_year                    1999
_chemical_formula_sum            'C106 H97 F12 N18 Ni O2.5 P2'
_chemical_formula_weight         2011.67
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.44(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.705(8)
_cell_length_b                   16.855(2)
_cell_length_c                   25.917(4)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.01
_cell_measurement_theta_min      4.82
_cell_volume                     9856(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0824
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9717
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        12.71
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.6807
_exptl_absorpt_correction_T_min  0.6544
_exptl_absorpt_correction_type   'emprical psi-scan'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             4180
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.181
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         8347
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.099
_refine_ls_restrained_S_obs      1.190
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_obs          0.0720
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2258
_refine_ls_wR_factor_obs         0.1735
_reflns_number_observed          4488
_reflns_number_total             8372
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901835Bsup1.cif
_cod_data_source_block           s6
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9855.5(40)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_original_formula_sum        'C106 H97 F12 N18 Ni O2.50 P2'
_cod_database_code               7027361