Crystallization of (012) oriented calcite single crystals underneath monolayers of tetra(carboxymethoxy)calix[4]arenes
Volkmer, Dirk; Fricke, Marc; Vollhardt, Dieter; Siegel, Stefan; Journal of the Chemical Society, Dalton Transactions  (2002) 4547–; doi:10.1039/b206912a

data_7012022
_publ_section_title
;
 Crystallization of (012) oriented calcite single crystals underneath
 monolayers of tetra(carboxymethoxy)calix[4]arenes
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4547
_journal_paper_doi               10.1039/b206912a
_journal_year                    2002
_chemical_formula_sum            'C72.75 H115.5 O17'
_chemical_formula_weight         1262.15
_chemical_name_systematic
; 
5,11,17,23-tetrakis-(1,1,3,3-tetramethylbutyl)-25,26,27,28-
tetra(carboxymethoxy)calix[4]arene 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                97.2510(10)
_cell_angle_beta                 93.3370(10)
_cell_angle_gamma                107.2020(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2924(5)
_cell_length_b                   12.8365(5)
_cell_length_c                   25.2557(11)
_cell_measurement_reflns_used    6131
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      26.94
_cell_measurement_theta_min      2.16
_cell_volume                     3757.2(3)
_computing_cell_refinement       'Bruker AXS SAINT'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_molecular_graphics
'Crystal Impact: DIAMOND; Bruker AXS: SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker AXS SMART'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38412
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9938
_exptl_absorpt_correction_T_min  0.9696
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .08
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         16065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0956P)^2^+1.7806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.2007
_reflns_number_gt                9892
_reflns_number_total             16065
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b206912a.txt
_cod_data_source_block           frick
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C72.75 H115.50 O17'
_cod_database_code               7012022