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_7012023
_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            'C77 H121 Ca2 O17.5 S4.5'
_chemical_formula_weight         1551.17
_chemical_name_systematic
; 
? 
;
_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                102.6710(10)
_cell_angle_beta                 98.3260(10)
_cell_angle_gamma                102.8720(10)
_cell_formula_units_Z            4
_cell_length_a                   17.0762(5)
_cell_length_b                   20.4361(7)
_cell_length_c                   25.9349(8)
_cell_measurement_reflns_used    8137
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.47
_cell_volume                     8427.9(5)
_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 0.958
_diffrn_measured_fraction_theta_max 0.958
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56343
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.06
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  0.9131
_exptl_absorpt_correction_T_min  0.8865
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3340
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.385
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1885
_refine_ls_number_reflns         35273
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.1199P)^2^+15.3047P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2108
_refine_ls_wR_factor_ref         0.2306
_reflns_number_gt                26347
_reflns_number_total             35273
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b206912a.txt
_cod_data_source_block           fricko2
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C77 H121 Ca2 O17.50 S4.50'
_cod_database_code               7012023