Structural Characterization of [(2,6-Pri2C6H3)NC(Me)C(H)C(Me)N(2,6-Pri2C6H3)K.PhCH3]\ιnfty: A Heavy Alkali Metal Diazapentadienyl Complex
William Clegg; Elaine K. Cope; Andrew J. Edwards; Francis S. Mair; Inorganic Chemistry 37 (1998) 2317–2319; doi:10.1021/ic970956j

data_4322765
_publ_section_title
;
 Structural Characterization of
 [(2,6-Pri2C6H3)NC(Me)C(H)C(Me)N(2,6-Pri2C6H3)K.PhCH3]\\infty: A Heavy
 Alkali Metal Diazapentadienyl Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2317
_journal_page_last               2319
_journal_paper_doi               10.1021/ic970956j
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C36 H49 K N2'
_chemical_formula_weight         548.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.137(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6537(9)
_cell_length_b                   26.200(2)
_cell_length_c                   11.9055(10)
_cell_measurement_reflns_used    8285
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      1.90
_cell_volume                     3281.0(5)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20002
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0028(6)
_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   1.024
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_obs          0.0639
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+2.6330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1604
_refine_ls_wR_factor_obs         0.1375
_reflns_number_observed          4901
_reflns_number_total             7507
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970956j.cif
_cod_data_source_block           fsm09
_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^)+(0.0587P)^2^+2.6330P] 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^)+(0.0587P)^2^+2.6330P] 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        3280.9(5)
_cod_database_code               4322765