4-Chlorobenzoyl-<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) o976–o977; doi:10.1107/S1600536812007003

data_2234491
_publ_section_title
;
 4-Chlorobenzoyl-<i>meso</i>-octamethylcalix[2]pyrrolidino[2]pyrrole: an
 acyl chloride derivative of a partially reduced calix[4] pyrrole
;
_journal_coeditor_code           ZQ2154
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o976
_journal_page_last               o977
_journal_paper_doi               10.1107/S1600536812007003
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C35 H47 Cl N4 O'
_chemical_formula_sum            'C35 H47 Cl N4 O'
_chemical_formula_weight         575.22
_chemical_melting_point          501
_chemical_name_common
;
4-Chlorobenzoyl-<i>meso</i>-octamethylcalix[2]pyrrolidino[2]pyrrole
;
_chemical_name_systematic
;
21-[(4-chlorophenyl)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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.798(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3224(6)
_cell_length_b                   12.0389(4)
_cell_length_c                   25.3311(13)
_cell_measurement_reflns_used    16706
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      1.62
_cell_volume                     3125.8(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       '\f + \w 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  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0565
_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       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32665
_diffrn_reflns_theta_full        25.63
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULscanABS in PLATON; Spek, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.344
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5906
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.1416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                4215
_reflns_number_total             5906
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zq2154.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2234491
_cod_database_fobs_code          2234491