Synthesis and characterization of two novel tetranuclear sodium ketoiminate complexes; structural evidence for formation of dative Na · · · F and Na‒C (olefin) bonding interactions
Chi, Yun; Ranjan, Sudhir; Chung, Po-Wen; Liu, Chao-Shiuan; Peng, Shie-Ming; Lee, Gene-Hsiang; Journal of the Chemical Society, Dalton Transactions  (2000) 343–; doi:10.1039/a908328f

data_7009043
_publ_section_title
;
 Synthesis and characterization of two novel tetranuclear sodium
 ketoiminate complexes; structural evidence for formation of dative
 Na&#x200A;&#x200A;&#x00B7;&#x2005;&#x00B7;&#x2005;&#x00B7;&#x200A;&#x200A;F
 and Na--C (olefin) bonding interactions
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              343
_journal_paper_doi               10.1039/a908328f
_journal_year                    2000
_chemical_formula_sum            'C32 H24 F24 N4 Na4 O4'
_chemical_formula_weight         1076.51
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 113.605(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6765(2)
_cell_length_b                   21.6103(2)
_cell_length_c                   16.0552(3)
_cell_measurement_reflns_used    6143
_cell_measurement_temperature    150(2)
_cell_volume                     4348.13(12)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19511
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.8238
_exptl_absorpt_correction_type   ' empirical used sadabs'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'irregular b'
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.120
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.120
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_obs          0.0564
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+5.0066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1374
_refine_ls_wR_factor_obs         0.1222
_reflns_number_observed          6107
_reflns_number_total             8771
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908328f.txt
_cod_data_source_block           compound2
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+5.0066P] 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^)+(0.0476P)^2^+5.0066P] 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        4348.13(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009043