Synthesis and crystal structure determination of two monomeric alkali metal phosphide derivatives: [M{P(H)C6H2-t-Bu3-2,4,6}(18-crown-6)] (M = K or Rb)
Rabe, Gerd W.; Heise, Henrike; Liable-Sands, Louise M.; Guzei, Ilia A.; Rheingold, Arnold L.; Journal of the Chemical Society, Dalton Transactions  (2000) 1863–; doi:10.1039/b000653j

data_7009398
_publ_section_title
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 Synthesis and crystal structure determination of two monomeric alkali
 metal phosphide derivatives: [M{P(H)C6H2-t-Bu3-2,4,6}(18-crown-6)]
 (M&#x2005;=&#x2005;K or Rb)
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1863
_journal_paper_doi               10.1039/b000653j
_journal_year                    2000
_chemical_formula_sum            'C30 H54 O6 P Rb'
_chemical_formula_weight         627.17
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 106.2640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.3994(5)
_cell_length_b                   9.16400(10)
_cell_length_c                   19.2861(2)
_cell_measurement_temperature    173(2)
_cell_volume                     6854.37(14)
_computing_cell_refinement       Siemens/SAINT
_computing_data_collection       Siemens/SMART
_computing_data_reduction        Siemens/SAINT
_computing_molecular_graphics    XP-5.03
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'phi, omega'
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10877
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    1.527
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6965
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_obs          0.0530
_refine_ls_shift/esd_max         -0.033
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1781
_refine_ls_wR_factor_obs         0.1449
_reflns_number_observed          5108
_reflns_number_total             6972
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000653j.txt
_cod_data_source_block           raba
_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^)+(0.1000P)^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^)+(0.1000P)^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        6854.36(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009398