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_7011118
_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            'C36 H66 Mn2 N8 Na2 O18'
_chemical_formula_weight         1054.82
_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
;
all carbon bonded H-atoms were placed at calculated positions, and the
hydroxyl H-atom on the two non-disorder methanol molecules were located
from a difference-Fourier map. No H-atoms were calculated for the disordered
methanol molecule.
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difference-Fourier
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.16(4)
_cell_angle_beta                 107.27(3)
_cell_angle_gamma                106.27(3)
_cell_formula_units_Z            1
_cell_length_a                   10.094(3)
_cell_length_b                   11.423(5)
_cell_length_c                   12.613(3)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      15
_cell_volume                     1245.0(9)
_computing_cell_refinement       'Stadi4 (Stoe & Cie, 1997a)'
_computing_data_collection       'Stadi4 (Stoe & Cie, 1997a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1997b)'
_computing_molecular_graphics    'SHELXTL/PC version 5.03 (Sheldrick, 1995)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       '\w-\q profile fitting'
_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  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0106
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4395
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        'variation +/- 2'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   'Psi scans'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'trigonal prism'
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.85
_refine_diff_density_min         -0.53
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment
;
riding model for the C-bonded H-atoms; isotropic refinement for the hydroxyl
H-atoms
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4381
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+2.4064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                4058
_reflns_number_total             4402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107873a.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+2.4064P] 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^)+(0.0718P)^2^+2.4064P] 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 
;
_cod_original_cell_volume        1245.0(7)
_cod_database_code               7011118