Structure Determination of Unsolvated Potassium, Rubidium, and Cesium Carbazolates
Dinnebier, Robert; Esbak, Hoda; Olbrich, Falk; Behrens, Ulrich; Organometallics 26 (2007) 2604–; doi:10.1021/om060927t

data_4072667
_publ_section_title
;
 Structure Determination of Unsolvated Potassium, Rubidium, and Cesium
 Carbazolates
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2604
_journal_paper_doi               10.1021/om060927t
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'laboratory preparation'
_chemical_formula_analytical     'C12 H8 K N'
_chemical_formula_moiety         'C12 H8 K N'
_chemical_formula_structural     '[K(NC12H8)]n'
_chemical_formula_sum            'C12 H8 K N'
_chemical_formula_weight         205.30
_chemical_melting_point          552.15
_chemical_name_common            'potassium carbazolate'
_chemical_name_systematic        ' potassium carbazolate'
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_audit_creation_date             2006-02-15T11:59
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
' 2006-02-15T11:59  Initial CIF as created by GSAS2CIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_formula_units_Z            18
_cell_length_a                   25.0827(9)
_cell_length_b                   25.0827
_cell_length_c                   7.83554(24)
_cell_measurement_temperature    100
_cell_volume                     4269.2(2)
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1998)'
_computing_structure_refinement  GSAS
_computing_structure_solution    'DASH structure solution package'
_diffrn_ambient_temperature      100
_diffrn_measurement_device_type  'StadiP, Stoe & Cie GmbH'
_diffrn_radiation_monochromator  Ge(111)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54056
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1908
_pd_block_id
2006-02-15T11:59|KCARBRV_NEW_RENAMED|R.E.D.|Stoe_Stadi-P
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  colourless
_pd_char_particle_morphology     'not determined'
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        60.09
_pd_meas_2theta_range_min        4.0
_pd_meas_number_of_points        5610
_pd_meas_scan_method             step
_pd_phase_name                   'K-carbazolid T= 100 K'
_pd_prep_temperature             100
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        60.05699
_pd_proc_2theta_range_min        3.96699
_pd_proc_info_datetime           2006-02-15T11:59:43
_pd_proc_info_excluded_regions   ' ?'
_pd_proc_ls_background_function
;   GSAS Background function number 2 with  4 terms.
 Cosine Fourier series
      1:    0.00000     2:    0.00000     3:    0.00000     4:    0.00000    
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_ls_profile_function
;
 CW Profile function number 4 with  16 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 Microstrain broadening by P.W. Stephens,  (1999). J. Appl. Cryst.,32,281-289.
 Peak tails are ignored  where the intensity is below 0.0010 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0442
_pd_proc_ls_prof_wR_expected     0.0726
_pd_proc_ls_prof_wR_factor       0.0562
_pd_proc_number_of_points        5610
_pd_spec_mounting                ' ?'
_refine_ls_goodness_of_fit_all   0.90
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_restraints     74
_refine_ls_R_Fsqd_factor         0.09915
_refine_ls_shift/su_max          0.09
_refine_ls_shift/su_mean         0.06
_reflns_d_resolution_high        1.543
_reflns_d_resolution_low         12.541
_reflns_limit_h_max              13
_reflns_limit_h_min              1
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              4
_reflns_limit_l_min              -5
_reflns_number_total             138
_cod_data_source_file            om060927trom20061010_045140.cif
_cod_data_source_block           KCarb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '279 oC' was changed to '552.15' - it
was converted from degrees Celsius(C) to
Kelvins(K).

'_geom_bond_publ_flag' value 'N' changed to 'n'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (46
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (63 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 
;
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4072667
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000