Syntheses and structures of structurally diverse potassium β-diketiminates derived from the ligand [{N(SiMe~3~)C(Ph)}~2~CH]^-^
Hitchcock, Peter B.; Lappert, Michael F.; Liu, Diang-Sheng; Sablong, Rafaël; Chemical Communications  (2002) 1920–1921; doi:10.1039/b205296b

data_7114467
_publ_section_title
;
 Syntheses and structures of structurally diverse potassium
 \b-diketiminates derived from the ligand
 [{N(SiMe~3~)C(Ph)}~2~CH]^-^
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1920
_journal_page_last               1921
_journal_paper_doi               10.1039/b205296b
_journal_year                    2002
_chemical_formula_structural     '[K(thf)2(Me3SiNCPhCHCPhNSiMe3)]n'
_chemical_formula_sum            'C29 H45 K N2 O2 Si2'
_chemical_formula_weight         548.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.05(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.217(3)
_cell_length_b                   19.020(3)
_cell_length_c                   15.526(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      14
_cell_volume                     3307.7(12)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      253(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6061
_diffrn_reflns_theta_max         65.95
_diffrn_reflns_theta_min         3.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.289
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.015
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_obs          0.0693
_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^)+(0.0815P)^2^+2.8932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2055
_refine_ls_wR_factor_obs         0.1674
_reflns_number_observed          3500
_reflns_number_total             5756
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b205296b.txt
_cod_data_source_block           mfl-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+2.8932P] 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^)+(0.0815P)^2^+2.8932P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114467