Zeolite-like crystal structure of an empty microporous molecular framework
Kepert, Cameron J.; Rosseinsky, Matthew J.; Chemical Communications  (1999) 375–; doi:10.1039/a809746a

data_7115199
_publ_contact_author
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      Matthew J. Rosseinsky
      Inorganic Chemistry Laboratory
      University of Oxford
      South Parks Road
      Oxford OX1 3QR
      UK
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_publ_section_title
;
 Zeolite-like crystal structure of an empty microporous molecular
 framework
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_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              375
_journal_paper_doi               10.1039/a809746a
_journal_year                    1999
_chemical_formula_moiety         'C15 H12 N5 Ni O6'
_chemical_formula_sum            'C15 H12 N5 Ni O6'
_chemical_formula_weight         417.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      68
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.883(1)
_cell_length_b                   19.049(1)
_cell_length_c                   17.415(1)
_cell_measurement_reflns_used    6655
_cell_measurement_temperature    375(2)
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      2.33
_cell_volume                     3942.0(5)
_computing_cell_refinement       'HKL (Otwinowski & Minor, 1996)'
_computing_data_collection       'XPRESS (MAC Science, 1989)'
_computing_data_reduction        'HKL (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    XPMA/ZORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_environment      'In an open 0.5 mm Lindemann tube'
_diffrn_ambient_temperature      375(2)
_diffrn_crystal_treatment
;
 A single crystal of [Ni(bpy)1.5(NO3)2].(EtOH) was warmed to 375 K (the
 desolvation temperature) at 20 K/hr. The crystal lay inside an open-ended
 capillary, itself immersed in a variable temperature dry nitrogen stream,
 throughout the experiment. 
;
_diffrn_detector                 'Eu/Ba image plate'
_diffrn_measurement_device       'Enraf-Nonius DIP2000 diffractometer'
_diffrn_measurement_method       'Ninety 2-degree oscillations in phi'
_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  0.039
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14645
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent blocks'
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.105
_refine_ls_goodness_of_fit_obs   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_restrained_S_obs      1.211
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_obs          0.0676
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1275P)^2^+4.7945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2210
_refine_ls_wR_factor_obs         0.2085
_reflns_number_observed          1480
_reflns_number_total             1958
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809746a.txt
_cod_data_source_block           Ni2(4,4'-bpy)3(NO3)4
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1275P)^2^+4.7945P] 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^)+(0.1275P)^2^+4.7945P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      Ccca
_cod_database_code               7115199