Synthesis and X-ray structure of [(THF)K(C5H4CH2CH2PPh2)]∞: a structurally characterized heavier alkali metal phosphane complex
Karsch, Hans H.; Graf, Volker W.; Reisky, Manfred; Chemical Communications  (1999) 1695–; doi:10.1039/a904248b

data_7110609
_publ_section_title
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 Synthesis and X-ray structure of [(THF)K(C5H4CH2CH2PPh2)]\\infty : a
 structurally characterized heavier alkali metal phosphane complex
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_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1695
_journal_paper_doi               10.1039/a904248b
_journal_year                    1999
_chemical_formula_moiety         'C23 H26 K O P'
_chemical_formula_sum            'C23 H26 K O P'
_chemical_formula_weight         388.51
_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                 90.56(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.432(1)
_cell_length_b                   19.929(1)
_cell_length_c                   10.026(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    199(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      9
_cell_volume                     2084.3(3)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        'CADSHEL V3.10 (Kopf, R\"ubcke, 1993)'
_computing_molecular_graphics    'SHELXTL(TM) PC'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      199(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       omega/theta
_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  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4763
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        6.13
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.340
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.065
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.065
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_obs          0.0363
_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^)+(0.0412P)^2^+0.9816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0993
_refine_ls_wR_factor_obs         0.0853
_reflns_number_observed          3285
_reflns_number_total             4529
_reflns_observed_criterion       >4sigma(I)
_cod_data_source_file            904248bsup1.cif
_cod_data_source_block           iogra1
_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^)+(0.0412P)^2^+0.9816P] 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^)+(0.0412P)^2^+0.9816P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7110609