Three Complexes of a [2.2]Cryptahemispherand
Maverick, Emily F.; Knobler, Carolyn B.; Trueblood, Kenneth N.; Ho, Siew Peng; Acta Crystallographica Section C 53 (1997) 1822–1827; doi:10.1107/S0108270197009530

data_2006794
_publ_section_title
;
 Three Complexes of a [2.2]Cryptahemispherand
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1822
_journal_page_last               1827
_journal_paper_doi               10.1107/S0108270197009530
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[K (C38 H52 N2 O7)] SCN , H2 O'
_chemical_formula_sum            'C39 H54 K N3 O8 S'
_chemical_formula_weight         764.01
_chemical_name_systematic
;36,37,38-Trimethoxy-5,10,15-trimethyl-22,25,30,33-tetraoxa-1,19-diazapentacyclo
 [17.8.8.1^3,7^.1^8,12^.1^13,17^]octatriaconta-3,5,7(36),8,10,12(37),13,15,
 17(38)-nonaene potassium thiocyanate monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.74(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.921(12)
_cell_length_b                   11.397(11)
_cell_length_c                   25.53(2)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    156
_cell_measurement_theta_max      8.8
_cell_measurement_theta_min      4.7
_cell_volume                     3966(6)
_computing_cell_refinement       'LEAST (UCLA Crystallographic Package, 1984)'
_computing_data_collection       'UCLA Crystallographic Package (1984)'
_computing_data_reduction
'CARESS (UCLA Crystallographic Package, 1984)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1995)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      156
_diffrn_measurement_device       'modified Picker FACS-1 (Crystal Logic)'
_diffrn_measurement_method       'profiles from \q/2\q 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  0.0821
_diffrn_reflns_av_sigmaI/netI    0.1550
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7045
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        'about 2'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_hydrogen_treatment
; H atoms riding; fixed C-H distances, <U^2^>~H~ = 1.2U~eq~(C),
  except for CH~3~ groups, for which factor was 1.5;
  CH~3~ groups rotating about C-C or O-C bond
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6763
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.120
_refine_ls_R_factor_all          0.2244
_refine_ls_R_factor_obs          .0642
_refine_ls_shift/esd_max         0.16
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0167P)^2^+12.2089P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2179
_refine_ls_wR_factor_obs         .1300
_reflns_number_observed          2462
_reflns_number_total             6768
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1279.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'No' changed to 'no' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (110 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'No' changed to 'no' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (110
times).

'_geom_angle_publ_flag' value 'No' changed to 'no' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (124
times).

'_geom_torsion_publ_flag' value 'No' changed to 'no'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (105
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0167P)^2^+12.2089P] where P = (Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0167P)^2^+12.2089P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2006794