An Na^+^ Complex and a Bis-BH~3~ Complex of a [1.1]Cryptahemispherand
Knobler, Carolyn B.; Maverick, Emily F.; Trueblood, Kenneth N.; Ho, Siew Peng; Acta Crystallographica Section C 53 (1997) 1827–1832; doi:10.1107/S0108270197009566

data_2006800
_publ_section_title
;
 An Na^+^ Complex and a Bis-BH~3~ Complex of a [1.1]Cryptahemispherand
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1827
_journal_page_last               1832
_journal_paper_doi               10.1107/S0108270197009566
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          'C34 H50 B2 N2 O5 , 0.5C1 H2 Cl2'
_chemical_formula_sum            'C34.5 H51 B2 Cl N2 O5'
_chemical_formula_weight         630.84
_chemical_name_systematic
;
hexahydro-{(30,31,32-trimethoxy-5,10,15-
trimethyl-22,27-dioxa-1,19-diazapentacyclo[17.5.5.1^3,7^.1^8,12^.1^13,17^]
dotriaconta-3,5,7(32),8,10,12(31),13,15,17(30)-nonaene-N^1^:N^19^)}
-di-boron    (CH~2~Cl~2~ solvate)
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_cell_angle_alpha                90.00(4)
_cell_angle_beta                 94.43(5)
_cell_angle_gamma                90.00(5)
_cell_formula_units_Z            4
_cell_length_a                   15.605(11)
_cell_length_b                   15.799(7)
_cell_length_c                   15.023(7)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      11.0
_cell_measurement_theta_min      7.5
_cell_volume                     3693(4)
_computing_cell_refinement       'Syntex (Crystal Logic) system'
_computing_data_collection       'Syntex (Crystal Logic) system'
_computing_data_reduction        '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      115(2)
_diffrn_measurement_device       'Syntex (Crystal Logic)'
_diffrn_measurement_method       \q/2\q
_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    0.1165
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7056
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        14
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.287
_refine_ls_extinction_coef       0.0007(5)
_refine_ls_extinction_method     'SHELXL93 (Xheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.193
_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     445
_refine_ls_number_reflns         5680
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.034
_refine_ls_restrained_S_obs      1.193
_refine_ls_R_factor_all          0.135
_refine_ls_R_factor_obs          .077
_refine_ls_shift/esd_max         0.335
_refine_ls_shift/esd_mean        0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.183
_refine_ls_wR_factor_obs         .158
_reflns_number_observed          3340
_reflns_number_total             6803
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1282.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 (50 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 (50
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 (74
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^)+(0.0704P)^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^)+(0.0704P)^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_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C34.5 H51 B2 Cl1 N2 O5'
_cod_database_code               2006800