Bis(1 degree-amino)cyclodistib(III)azanes: the first structural characterization of cis and trans isomers of a single cyclodipnict(III)azane.
Eisler, Dana J.; Chivers, Tristram; Inorganic chemistry 45 (2006) 10734–10742; doi:10.1021/ic061660t

data_4350622
_publ_section_title
;
 Bis(1 degree-amino)cyclodistib(III)azanes: the first structural
 characterization of cis and trans isomers of a single
 cyclodipnict(III)azane.
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10734
_journal_page_last               10742
_journal_paper_doi               10.1021/ic061660t
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C24 H52 N4 Na2 O2 Sb2'
_chemical_formula_sum            'C24 H52 N4 Na2 O2 Sb2'
_chemical_formula_weight         718.18
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.305(4)
_cell_length_b                   16.439(3)
_cell_length_c                   11.772(2)
_cell_measurement_temperature    173(2)
_cell_volume                     3348.9(11)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi\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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21640
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.663
_exptl_absorpt_correction_T_max  0.8784
_exptl_absorpt_correction_T_min  0.7321
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.678
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3951
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+4.5306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                3168
_reflns_number_total             3951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061660tsi20060901_013006.cif
_cod_data_source_block           complex5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3349.0(12)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4350622