Bowl-shaped Cu(I) metallamacrocyclic ethylene and carbonyl adducts as structural analogues of organic calixarenes.
Maekawa, Masahiko; Konaka, Hisashi; Minematsu, Toshie; Kuroda-Sowa, Takayoshi; Munakata, Megumu; Kitagawa, Susumu; Chemical communications (Cambridge, England)  (2007) 5179–5181; doi:10.1039/b713618h

data_7102379
_publ_section_title
;
 Bowl-shaped Cu(I) metallamacrocyclic ethylene and carbonyl adducts as
 structural analogues of organic calixarenes.
;
_journal_issue                   48
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5179
_journal_page_last               5181
_journal_paper_doi               10.1039/b713618h
_journal_year                    2007
_chemical_formula_moiety         'C33 H33 Cu3 N9, 3(Cl O4)'
_chemical_formula_sum            'C33 H33 Cl3 Cu3 N9 O12'
_chemical_formula_weight         1044.67
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   14.4419(7)
_cell_length_b                   38.607(2)
_cell_length_c                   21.448(1)
_cell_measurement_reflns_used    30713
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     11958(1)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       12
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            93735
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.860
_exptl_absorpt_correction_T_max  0.757
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             6336.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.54
_refine_ls_abs_structure_details 'Flack(1983), 9136 Friedel pairs'
_refine_ls_abs_structure_Flack   0.113(9)
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     1621
_refine_ls_number_reflns         23226
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          -0.0030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0428P)^2^+17.0296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                19520
_reflns_number_total             23226
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b713618h.txt
_cod_data_source_block
'[Cu3(pprd)3(C2H4)3]3(ClO4)9_Complex4-CCDC-659371'
_cod_original_sg_symbol_Hall     'P 2c -2n '
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C33 H33 Cl3 Cu3 N9 O12 '
_cod_database_code               7102379