Na±Mediated aggregation of imino-carboxylate transition metal complexes
Dan M. J. Doble; Alexander J. Blake; Wan-Sheung Li; Martin Schröder; J. Chem. Soc., Dalton Trans.  (2001) 3137–3139; doi:10.1039/b107873a

data_7011120
_publ_section_title
;
 Na+-Mediated aggregation of imino-carboxylate transition metal
 complexes
;
_journal_issue                   21
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3137
_journal_page_last               3139
_journal_paper_doi               10.1039/b107873a
_journal_year                    2001
_chemical_formula_sum            'C15 H21 B F4 N4 Na2 Ni O6'
_chemical_formula_weight         544.86
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens
'Me Hs found in delta-F, -CH2- placed geometrically'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier synthesis'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            4
_cell_length_a                   9.369(3)
_cell_length_b                   9.369(3)
_cell_length_c                   28.603(6)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.9
_cell_measurement_theta_min      14.05
_cell_volume                     2174.3(11)
_computing_cell_refinement       'STADI-4 (Stoe & Cie, 1996a)'
_computing_data_collection       'STADI-4 (Stoe & Cie, 1996a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       omega-theta
_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  0.1106
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4781
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        5.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.17
_refine_diff_density_min         -0.47
_refine_diff_density_rms         0.10
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         1284
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+3.7435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1749
_refine_ls_wR_factor_ref         0.1885
_reflns_number_gt                1111
_reflns_number_total             1284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107873a.txt
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+3.7435P] 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^)+(0.1128P)^2^+3.7435P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 

2024-03-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C30 H42 B2 F8 N8 Na4 Ni2 O12'
_cod_original_formula_weight         1089.72
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P31c
_cod_database_code               7011120