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_4508558
_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            'C129 H175 Cd2 N11 O32'
_chemical_formula_weight         2616.60
_chemical_name_common            '8 - PCH532 Cd A-DDBuC[4] TMEPhen'
_chemical_name_systematic
;
 ?
;
_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                79.620(5)
_cell_angle_beta                 74.012(3)
_cell_angle_gamma                63.599(3)
_cell_formula_units_Z            2
_cell_length_a                   17.7359(10)
_cell_length_b                   19.8660(15)
_cell_length_c                   21.1162(12)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.50
_cell_measurement_theta_min      2.45
_cell_volume                     6392.0(7)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       '\f and \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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            96526
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.9037
_exptl_absorpt_correction_T_min  0.8860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.802
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1497
_refine_ls_number_reflns         31621
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1829P)^2^+7.9254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2529
_refine_ls_wR_factor_ref         0.2811
_reflns_number_gt                22901
_reflns_number_total             31621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4013685_si_005.cif
_cod_data_source_block           8
_cod_depositor_comments
;

2021-04-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C258 H350 Cd4 N22 O64'
_cod_original_formula_weight         5233.20
_cod_original_formula_units_Z            1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4508558