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_2006793
_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          '[Na (C38 H52 N2 O7)]SCN'
_chemical_formula_sum            'C39 H52 N3 Na O7 S'
_chemical_formula_weight         729.89
_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 sodium thiocyanate clathrate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 117.89(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.907(6)
_cell_length_b                   12.543(4)
_cell_length_c                   20.860(7)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      10.4
_cell_volume                     3910(3)
_computing_cell_refinement       'Syntex P\=1 diffractometer software'
_computing_data_collection       'Syntex P\=1 diffractometer software'
_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    'YZARC (Declercq, Germain & Woolfson, 1979)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Syntex  P\=1'
_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  'not known'
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3875
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_meas      ?
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1556
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_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.251
_refine_ls_abs_structure_details 'Flack  (1983) parameter = 0.42(35)'
_refine_ls_abs_structure_Flack   0.4(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_obs   1.201
_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 bond
;
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_refine_ls_number_restraints     2
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_refine_ls_restrained_S_obs      1.200
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_obs          .0548
_refine_ls_shift/esd_max         0.468
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0717P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1516
_refine_ls_wR_factor_obs         .1354
_reflns_number_observed          2814
_reflns_number_total             3468
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1279.cif
_cod_data_source_block           I
_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 (72 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 (72
times).

'_geom_contact_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 (22
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 (70
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 (92
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^)+(0.0717P)^2^] 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^)+(0.0717P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3910(2)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2006793