5,7,7,12,14,14-Hexamethyl-4,11-diaza-1,8-diazoniacyclotetradecane pentacyanonitrosoferrate(II) dihydrate: a supramolecular compound constructed by hydrogen bonds
Ai-Hua Yuan; Xiao-Ping Shen; Hu Zhou; Acta Crystallographica Section C 62 (2006) m161–m162; doi:10.1107/S0108270105035146

data_2015222
_publ_section_title
;
 5,7,7,12,14,14-Hexamethyl-4,11-diaza-1,8-diazoniacyclotetradecane
 pentacyanonitrosoferrate(II) dihydrate: a supramolecular compound
 constructed by hydrogen bonds
;
_journal_coeditor_code           AV1254
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m161
_journal_page_last               m162
_journal_paper_doi               10.1107/S0108270105035146
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C16 H38 N4) [Fe (C N)5 (N O)], 2H2 O'
_chemical_formula_moiety         'C16 H38 N4 2+, C5 Fe N6 O 2-, 2H2 O1'
_chemical_formula_sum            'C21 H42 Fe N10 O3'
_chemical_formula_weight         538.50
_chemical_name_systematic
;
5,7,7,12,14,14-hexamethyl-4,11-diaza-1,8-diazoniacyclotetradecane
pentacyanonitrosoferrate(II)
;
_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           SHELXL-97
_cell_angle_alpha                74.525(2)
_cell_angle_beta                 78.926(2)
_cell_angle_gamma                70.318(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9527(12)
_cell_length_b                   10.7737(14)
_cell_length_c                   16.977(2)
_cell_measurement_reflns_used    1759
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.75
_cell_measurement_theta_min      2.43
_cell_volume                     1476.5(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7878
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.424
_refine_ls_extinction_coef       0.08(2)
_refine_ls_extinction_method     SHELXS97
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.4822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                3941
_reflns_number_total             5633
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            av1254.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_sg_symbol_H-M      'P -1   '
_cod_database_code               2015222
_cod_database_fobs_code          2015222