4-Methoxybenzoyl-<i>meso</i>-octamethylcalix[2]pyrrolidino[2]pyrrole: an acyl chloride derivative of a partially reduced calix[4]pyrrole
Journot, Guillaume; Neier, Reinhard; Stoeckli-Evans, Helen; Acta Crystallographica Section E 68 (2012) o929–o930; doi:10.1107/S1600536812008008

data_2234085
_publ_section_title
;
 4-Methoxybenzoyl-<i>meso</i>-octamethylcalix[2]pyrrolidino[2]pyrrole: an
 acyl chloride derivative of a partially reduced calix[4]pyrrole
;
_journal_coeditor_code           AA2052
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o929
_journal_page_last               o930
_journal_paper_doi               10.1107/S1600536812008008
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C36 H50 N4 O2'
_chemical_formula_moiety         'C36 H50 N4 O2'
_chemical_formula_sum            'C36 H50 N4 O2'
_chemical_formula_weight         570.80
_chemical_melting_point          488
_chemical_name_common
;
4-Methoxybenzoyl-meso-octamethylcalix[2]pyrrolidino[2]pyrrole
;
_chemical_name_systematic
;
21-[(4-methoxyphenyl)carbonyl]-2,2,7,7,12,12,17,17-octamethyl-21,22,23,24-
tetraazapentacyclo[16.2.1.1^3,6^.1^8,11^.1^13,16^]tetracosa-3,5,13,15-tetraene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.629(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3150(4)
_cell_length_b                   11.8104(5)
_cell_length_c                   26.1856(10)
_cell_measurement_reflns_used    22254
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      1.57
_cell_volume                     3153.9(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2009)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS II'
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33803
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.64
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS in PLATON; Spek, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.165
_refine_ls_extinction_coef       0.0016(3)
_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   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0447P)^2^+0.4659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                4470
_reflns_number_total             5943
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            aa2052.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2234085
_cod_database_fobs_code          2234085