4,6,12,14-Tetra-<i>tert</i>-butyl-17-<i>N</i>-(6-methylpyridin-2-yl)-8,16-dioxa-17-azatetracyclo[7.7.1.0^2,7^.0^10,15^]heptadeca-2,4,6,10,12,14-hexaene methanol solvate
Xu, Li; Kim, Youngmee; Qi, Xin; Kim, Sung-Jin; Acta Crystallographica Section E 62 (2006) o243–o245; doi:10.1107/S1600536805041383

data_2207925
_publ_section_title
;4,6,12,14-Tetra-<i>tert</i>-butyl-17-<i>N</i>-(6-methylpyridin-2-yl)-8,16-dioxa-17-azatetracyclo[7.7.1.0^2,7^.0^10,15^]heptadeca-2,4,6,10,12,14-hexaene
 methanol solvate
;
_journal_coeditor_code           WN6397
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o243
_journal_page_last               o245
_journal_paper_doi               10.1107/S1600536805041383
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C36 H48 N2 O2, C H4 O'
_chemical_formula_moiety         'C36 H48 N2 O2, C H4 O'
_chemical_formula_sum            'C37 H52 N2 O3'
_chemical_formula_weight         572.81
_chemical_name_systematic
;
4,6,12,14-Tetra-tert-butyl-17-N-(6-methylpyridin-2-yl)-8,16-dioxa-17-
azatetracyclo[7.7.1.0^2,7^.0^10,15^]heptadeca-2,4,6,10,12,14-hexaene
methanol solvate
;
_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                66.313(4)
_cell_angle_beta                 82.711(4)
_cell_angle_gamma                68.295(4)
_cell_formula_units_Z            2
_cell_length_a                   10.282(2)
_cell_length_b                   12.775(3)
_cell_length_c                   15.601(3)
_cell_measurement_reflns_used    877
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      18.51
_cell_measurement_theta_min      2.28
_cell_volume                     1743.0(6)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.2218
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9105
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.616
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.616
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0568P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                1913
_reflns_number_total             6047
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6397.cif
_cod_data_source_block           I
_cod_original_cell_volume        1743.0(7)
_cod_database_code               2207925
_cod_database_fobs_code          2207925