Complexation of stable carbenes with alkali metals
Alder, Roger W.; Blake, Michael E.; Bortolotti, Christel; Bufali, Simone; Butts, Craig P.; Linehan, Emma; Oliva, Josep M.; Guy Orpen, A.; Quayle, Michael J.; Chemical Communications  (1999) 241–; doi:10.1039/a808951e

data_7110410
_publ_section_title
;
 Complexation of stable carbenes with alkali metals
;
_journal_issue                   3
_journal_name_full               'Chemical Communications'
_journal_page_first              241
_journal_paper_doi               10.1039/a808951e
_journal_year                    1999
_chemical_formula_sum            'C32 H76 K2 N6 Si4'
_chemical_formula_weight         735.55
_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
_cell_angle_alpha                73.97(2)
_cell_angle_beta                 73.132(12)
_cell_angle_gamma                69.426(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4128(12)
_cell_length_b                   10.937(3)
_cell_length_c                   12.306(2)
_cell_measurement_reflns_used    130
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.75
_cell_volume                     1113.4(4)
_computing_cell_refinement       'SMART (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SMART (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995a)'
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11499
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0.14
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.887862
_exptl_absorpt_correction_T_min  0.774504
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       'Irregular Block'
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.988
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         5034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_obs          0.0266
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0762
_refine_ls_wR_factor_obs         0.0743
_reflns_number_observed          4058
_reflns_number_total             5034
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808951esup1.cif
_cod_data_source_block           kcarb
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0000P] 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^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1113.5(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110410