4,4',4''-(Methanetriyl)triphenyl tris(2,2,5,5-tetramethyl-1-oxyl-3-pyrroline-3-carboxylate) benzene trisolvate
Schuetz, Denise; Margraf, Dominik; Prisner, Thomas F.; Bats, Jan W.; Acta Crystallographica Section E 66 (2010) o729–o730; doi:10.1107/S1600536810007294

data_2225634
_publ_section_title
;
 4,4',4''-(Methanetriyl)triphenyl
 tris(2,2,5,5-tetramethyl-1-oxyl-3-pyrroline-3-carboxylate) benzene
 trisolvate
;
_journal_coeditor_code           LH5001
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o729
_journal_page_last               o730
_journal_paper_doi               10.1107/S1600536810007294
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C46 H52 N3 O9, 3C6 H6'
_chemical_formula_moiety         'C46 H52 N3 O9, 3(C6 H6)'
_chemical_formula_sum            'C64 H70 N3 O9'
_chemical_formula_weight         1025.23
_chemical_name_systematic
;
4,4',4''-(Methanetriyl)triphenyl
tris(2,2,5,5-tetramethyl-1-oxyl-3-pyrroline-3-carboxylate)
benzene trisolvate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.324(10)
_cell_angle_beta                 92.765(11)
_cell_angle_gamma                105.308(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0810(13)
_cell_length_b                   11.7372(16)
_cell_length_c                   26.241(4)
_cell_measurement_reflns_used    204
_cell_measurement_temperature    164(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     2951.0(7)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      164(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Siemens SMART 1K CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0876
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            43135
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  1200
_diffrn_standards_number         297
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1536
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.09P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1936
_reflns_number_gt                6172
_reflns_number_total             12901
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5001.cif
_cod_data_source_block           I
_cod_original_cell_volume        2951.1(7)
_cod_database_code               2225634
_cod_database_fobs_code          2225634