Blue Alkali Dinitrosomethanides: Synthesis, Structure, and Bonding
Harald Brand; Peter Mayer; Kurt Polborn; Axel Schulz; Jan J. Weigand; Journal of the American Chemical Society 127 (2005) 1360–1361; doi:10.1021/ja042877u

data_4111403
_publ_contact_author
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 Axel Schulz 
 Department Chemie
 Universit\"at M\"unchen
 Butenandtstr. 5-13 
 D-81377 M\"unchen
 Bundesrepublik Deutschland
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_publ_contact_author_email       lex@cup.uni-muenchen.de
_publ_contact_author_fax         '049 89 2180-77492'
_publ_contact_author_phone       '049 89 2180-77763'
_publ_section_title
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 Blue Alkali Dinitrosomethanides: Synthesis, Structure, and Bonding
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1360
_journal_page_last               1361
_journal_paper_doi               10.1021/ja042877u
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C12 H24 O6 K^+    C H N2 O2^-'
_chemical_formula_sum            'C13 H25 K N2 O8'
_chemical_formula_weight         376.45
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             11-Nov-04
_audit_creation_method           SHELXL
_audit_update_record             ' ?'
_cell_angle_alpha                90.00
_cell_angle_beta                 99.816(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2137(8)
_cell_length_b                   14.215(2)
_cell_length_c                   7.9909(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      9
_cell_volume                     919.3(2)
_computing_cell_refinement       CAD4(Nonius,_1977)
_computing_data_collection       CAD4(Nonius,_1977)
_computing_data_reduction        process_MOLEN(Fair,_1990)
_computing_molecular_graphics    ZORTEP(Zsolnai,Huttner,_1994)
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Nonius_MACH3
_diffrn_measurement_method       \o-2\T-scan
_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  0.0121
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2881
_diffrn_reflns_theta_full        23.97
_diffrn_reflns_theta_max         23.97
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        -0.3
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_correction_T_min  0.9576
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       plate
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.105
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2083
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.151
_refine_ls_restrained_S_obs      1.161
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_obs          0.0395
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.4169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1122
_refine_ls_wR_factor_obs         0.1033
_reflns_number_observed          1795
_reflns_number_total             2083
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja042877usi20041125_081728.cif
_cod_data_source_block           brand5b
_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^)+(0.0532P)^2^+0.4169P] 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^)+(0.0532P)^2^+0.4169P] 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_database_code               4111403