Enhancing Strategies for the Assembly of Metal‒Organic Systems with Inherent Cavity-Containing Calix[4]arenes
Cholewa, Piotr P.; Beavers, Christine M.; Teat, Simon J.; Dalgarno, Scott J.; Crystal Growth & Design 13 (2013) 5165–; doi:10.1021/cg4013685

data_4508559
_publ_section_title
;
 Enhancing Strategies for the Assembly of Metal--Organic Systems with
 Inherent Cavity-Containing Calix[4]arenes
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5165
_journal_paper_doi               10.1021/cg4013685
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C57 H65 Cd N5 O12'
_chemical_formula_weight         1124.54
_chemical_name_common            PCH469
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.8642(4)
_cell_length_b                   15.8642(4)
_cell_length_c                   42.9758(15)
_cell_measurement_reflns_used    9141
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.51
_cell_volume                     10815.8(5)
_computing_cell_refinement       'Bruker SAINT v7.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.34a'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXT (beta verion)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Apex II CCD Diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            76809
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.9544
_exptl_absorpt_correction_T_min  0.9544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2004 Bruker AXS, Manison, WI'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Square base pyramid'
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         10325
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1246P)^2^+4.4464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.1804
_reflns_number_gt                9279
_reflns_number_total             10325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4013685_si_006.cif
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      P43212
_cod_database_code               4508559