Monomeric Alkali Metal (Li, Na, K) Complexes of Bis(iminophosphorano)methanides
Kamalesh Babu, Ruppa P.; Aparna, Kasani; McDonald, Robert; Cavell, Ronald G.; Organometallics 20 (2001) 1451–; doi:10.1021/om000982g

data_4077255
_publ_section_title
;
 Monomeric Alkali Metal (Li, Na, K) Complexes of
 Bis(iminophosphorano)methanides
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1451
_journal_paper_doi               10.1021/om000982g
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C35 H73 Li N2 O P2 Si2'
_chemical_formula_weight         663.01
_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                 95.089(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4393(12)
_cell_length_b                   18.457(2)
_cell_length_c                   21.421(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      13.46
_cell_measurement_theta_min      12.27
_cell_volume                     4111.1(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7685
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.46
_diffrn_standards_interval_count 297
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  .8934
_exptl_absorpt_correction_T_min  .8465
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.45
_refine_diff_density_max         .454
_refine_diff_density_min         -.441
_refine_diff_density_rms         .056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7256
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_obs          0.0587
_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^)+( 0.0544P)^2^+3.1275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1450
_refine_ls_wR_factor_obs         0.1213
_reflns_number_observed          4638
_reflns_number_total             7258
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om000982g.cif
_cod_data_source_block           rgc9828_Compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0544P)^2^+3.1275P] 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^)+( 0.0544P)^2^+3.1275P] 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        4111.0(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077255