Two Isomeric [2.1]Cryptahemispherand Diamides
Maverick, Emily F.; Knobler, Carolyn B.; Trueblood, Kenneth N.; Ho, Siew Peng; Acta Crystallographica Section C 53 (1997) 1835–1838; doi:10.1107/S0108270197009554

data_2006797
_publ_section_title
;
 Two Isomeric [2.1]Cryptahemispherand Diamides
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1835
_journal_page_last               1838
_journal_paper_doi               10.1107/S0108270197009554
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C36 H44 N2 O8'
_chemical_formula_weight         632.73
_chemical_name_systematic
;33,34,35-Trimethoxy-5,10,15-trimethyl-22,25,30-trioxa-1,19-diazapentacyclo(17.8
 .5.1^3,7^,1^8,12^.1^13,17^)pentatriaconta-3,5,7(35),8,10,12(34),13,15,17(3
 3)-nonaene-2,18-dione
C36 H44 N2 O8
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_cell_angle_alpha                90.00(2)
_cell_angle_beta                 90.00(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   7.8350(14)
_cell_length_b                   37.230(8)
_cell_length_c                   11.318(3)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    117(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     3301.4(13)
_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    'MULTAN80 (Declercq et al., 1979)'
_diffrn_ambient_temperature      117(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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3733
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'nearly rectangular parallelepiped'
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.286
_refine_ls_abs_structure_details 'Flack (1983) parameter = 0.3 (19)'
_refine_ls_abs_structure_Flack   0.3(19)
_refine_ls_extinction_coef       0.0005(6)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.086
_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     422
_refine_ls_number_reflns         3733
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_obs          .0610
_refine_ls_shift/esd_max         -0.673
_refine_ls_shift/esd_mean        0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0627P)^2^+2.8088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1616
_refine_ls_wR_factor_obs         .1462
_reflns_number_observed          2933
_reflns_number_total             3733
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1281.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 (52 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 (52
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 (24
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 (80
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 (101
time).

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 'none' 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 'w =
1/[\s^2^(Fo^2^)+(0.0627P)^2^+2.8088P] 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^)+(0.0627P)^2^+2.8088P] 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      Pna2~1~
_cod_database_code               2006797