3,9-Dimethyl-3,9-bis(4-nitrophenyl)-2,4,8,10-tetraoxaspiro[5.5]undecane
Sun, Xiaoqiang; Yu, Bin; Zhang, Xiuqin; Chao, Xuqiang; Chen, Qiang; Acta Crystallographica Section E 67 (2011) o1319–; doi:10.1107/S1600536811015017

data_2230368
_publ_section_title
;
 3,9-Dimethyl-3,9-bis(4-nitrophenyl)-2,4,8,10-tetraoxaspiro[5.5]undecane
;
_journal_coeditor_code           IS2689
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1319
_journal_paper_doi               10.1107/S1600536811015017
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C21 H22 N2 O8'
_chemical_formula_moiety         'C21 H22 N2 O8'
_chemical_formula_sum            'C21 H22 N2 O8'
_chemical_formula_weight         430.41
_chemical_name_systematic
;
3,9-Dimethyl-3,9-bis(4-nitrophenyl)-2,4,8,10-tetraoxaspiro[5.5]undecane
;
_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                115.280(4)
_cell_angle_beta                 94.426(4)
_cell_angle_gamma                103.444(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4215(12)
_cell_length_b                   11.8790(18)
_cell_length_c                   13.522(3)
_cell_measurement_reflns_used    3502
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.20
_cell_measurement_theta_min      2.88
_cell_volume                     1027.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5588
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_correction_T_min  0.9757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3563
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1350P)^2^+0.1621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1866
_reflns_number_gt                2980
_reflns_number_total             3563
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is2689.cif
_cod_data_source_block           I
_cod_original_cell_volume        1027.0(3)
_cod_database_code               2230368
_cod_database_fobs_code          2230368