Triprotic 2,4,6-tris-organoamino-1,3,5-triazenes as precursor to multi-site triazenate ligands
Frederic Rivals; Alexander Steiner; Chemical Communications 20 (2001) 2104–2105; doi:10.1039/B105435J

data_7123810
_publ_section_title
;
 Triprotic 2,4,6-tris-organoamino-1,3,5-triazenes as precursor to
 multi-site triazenate ligands
;
_journal_name_full               'Chemical Communications'
_journal_page_first              2104
_journal_page_last               2105
_journal_paper_doi               10.1039/B105435J
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C76 H96 F6 Li4 N12 O7'
_chemical_formula_weight         1431.41
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                68.66(3)
_cell_angle_beta                 72.98(5)
_cell_angle_gamma                79.06(5)
_cell_formula_units_Z            1
_cell_length_a                   10.121(6)
_cell_length_b                   14.415(3)
_cell_length_c                   15.282(3)
_cell_measurement_temperature    200(2)
_cell_volume                     1977.0(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\w oscillation'
_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  0.1602
_diffrn_reflns_av_sigmaI/netI    0.1921
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7579
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.087
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             758
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         3514
_refine_ls_number_restraints     742
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.1630
_refine_ls_R_factor_gt           0.0947
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2311
_reflns_number_gt                1529
_reflns_number_total             3514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Chem-Comm-2001-20-2104.cif
_cod_data_source_block           B105435J
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1977.0(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7123810
_disorder_refine_details
;
C-positions of coordinated thf molecules were split in two positions and
refined with one occupancy factor per thf molecule using similar-distance
and similar-U restraints. The non-coordinated thf and hexane molecules
are located on inversion centres, where they are disordered over two
positions. Both were refined using similar-distance and similar-U
restraints. Non-disordered non-H-atoms were refined anisotropically.
Disordered non-H-atoms were refined isotropically.
;