7-Isopropylidene-<i>N</i>^2^,<i>N</i>^3^,<i>N</i>^5^,<i>N</i>^6^-tetramethoxy-<i>N</i>^2^,<i>N</i>^3^,<i>N</i>^5^,<i>N</i>^6^-tetramethylbicyclo[2.2.1]hepta-2,5-diene-2,3,5,6-tetracarboxamide
Sahlmann, Benjamin; Näther, Christian; Herges, Rainer; Acta Crystallographica Section E 70 (2014) o438–; doi:10.1107/S1600536814004255

data_2239211
_publ_section_title
;
 7-Isopropylidene-<i>N</i>^2^,<i>N</i>^3^,<i>N</i>^5^,<i>N</i>^6^-tetramethoxy-<i>N</i>^2^,<i>N</i>^3^,<i>N</i>^5^,<i>N</i>^6^-tetramethylbicyclo[2.2.1]hepta-2,5-diene-2,3,5,6-tetracarboxamide
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o438
_journal_paper_doi               10.1107/S1600536814004255
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C22 H32 N4 O8'
_chemical_formula_moiety         'C22 H32 N4 O8'
_chemical_formula_sum            'C22 H32 N4 O8'
_chemical_formula_weight         480.52
_chemical_name_systematic
7-Isopropylidene-<i>N</i>^2^,<i>N</i>^3^,<i>N</i>^5^,<i>N</i>^6^-tetramethoxy-<i>N</i>^2^,<i>N</i>^3^,<i>N</i>^5^,<i>N</i>^6^-tetramethylbicyclo[2.2.1]hepta-2,5-diene-2,3,5,6-tetracarboxamide
_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                94.648(12)
_cell_angle_beta                 91.548(13)
_cell_angle_gamma                108.013(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5830(9)
_cell_length_b                   10.2662(8)
_cell_length_c                   13.3792(16)
_cell_measurement_reflns_used    3915
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      4
_cell_volume                     1245.7(2)
_computing_cell_refinement       '<i>X-AREA</i> (Stoe & Cie, 2008)'
_computing_data_collection       '<i>X-AREA</i> (Stoe & Cie, 2008)'
_computing_data_reduction        '<i>X-AREA</i> (Stoe & Cie, 2008)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       'Phi 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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10017
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.186
_refine_ls_extinction_coef       0.079(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0701P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                3431
_reflns_number_total             4788
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2450sup1.cif
_cod_data_source_block           I
_cod_database_code               2239211
_cod_database_fobs_code          2239211