Bis(μ-18-nitro-2,3,5,6,8,9,11,12,14,15-decahydro-1,4,7,10,13,16-benzohexaoxacyclooctadecine)bis[(chlorochromato)potassium]
Kotlyar, Sergei A.; Shishkina, Svetlana V.; Shishkin, Oleg V.; Pluzhnik-Gladyr, Sergei M.; Kiriyak, Andrey V.; Chuprin, Gennady N.; Kamalov, Gerbert L.; Acta Crystallographica Section E 62 (2006) m1988–m1989; doi:10.1107/S1600536806026511

data_2209932
_publ_section_title
Bis(\m-18-nitro-2,3,5,6,8,9,11,12,14,15-decahydro-1,4,7,10,13,16-benzohexaoxacyclooctadecine)bis[(chlorochromato)potassium]
_journal_coeditor_code           LH2118
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1988
_journal_page_last               m1989
_journal_paper_doi               10.1107/S1600536806026511
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[K (C16 H23 N1 O8)] [Cr Cl O3]'
_chemical_formula_moiety         'C16 H23 N1 O7 + , Cl Cr O3 -'
_chemical_formula_sum            'C16 H23 Cl Cr K N O11'
_chemical_formula_weight         531.91
_chemical_name_systematic
;bis[(18-nitro-2,3,5,6,8,9,11,12,14,15-
decahydro-1,4,7,10,13,16-benzohexaoxacyclooctadecine)potassium
 chlorochromate]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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           SHELXL97
_cell_angle_alpha                100.959(9)
_cell_angle_beta                 98.728(9)
_cell_angle_gamma                98.782(9)
_cell_formula_units_Z            2
_cell_length_a                   8.7780(10)
_cell_length_b                   9.5310(10)
_cell_length_c                   13.6780(10)
_cell_measurement_reflns_used    3015
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34
_cell_measurement_theta_min      3
_cell_volume                     1090.9(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'XP (Siemens, 1998)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  SHELXTL/PC
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Oxford Xcalibur3'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.079
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8636
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.94
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       transparent
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.289
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.087
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0655P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.105
_refine_ls_wR_factor_ref         0.114
_reflns_number_gt                2363
_reflns_number_total             3715
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2118.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1090.8(2)
_cod_original_formula_sum        'C16 H23 Cl1 Cr1 K1 N1 O11'
_cod_database_code               2209932
_cod_database_fobs_code          2209932