Synthesis and structure of [Cp2PbCpthf Na]·0.5thf; implications to the control of dimensionality in p block metallocene anion systems (Cp = C5H5, Cpthf = {C5H4}CH2C4H7O)
Feeder, Neil; Hopkins, Alexander D.; Layfield, Richard A.; Wright, Dominic S.; Journal of the Chemical Society, Dalton Transactions  (2000) 2247–; doi:10.1039/b004608f

data_7009950
_publ_section_title
;
 Synthesis and structure of
 [Cp2PbCpthf&#x200A;&#x200A;Na]&#x00B7;0.5thf; implications to the
 control of dimensionality in p block metallocene anion systems
 (Cp&#x2005;=&#x2005;C5H5, Cpthf&#x2005;=&#x2005;{C5H4}CH2C4H7O)
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2247
_journal_paper_doi               10.1039/b004608f
_journal_year                    2000
_chemical_formula_sum            'C22.5 H28 Na O1.5 Pb'
_chemical_formula_weight         552.63
_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                 92.230(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1145(8)
_cell_length_b                   15.798(2)
_cell_length_c                   15.0060(10)
_cell_measurement_temperature    150(2)
_cell_volume                     2159.1(4)
_computing_cell_refinement       maXus
_computing_data_collection       maXus
_computing_data_reduction        maXus
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    SIR
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       NoniusKappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10002
_diffrn_reflns_theta_max         22.45
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    7.844
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_F_000             1072
_refine_diff_density_max         1.661
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         2788
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_obs          0.0676
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+37.3805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1950
_refine_ls_wR_factor_obs         0.1786
_reflns_number_observed          2252
_reflns_number_total             2798
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004608f.txt
_cod_data_source_block           dw0009
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+37.3805P] 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^)+(0.0986P)^2^+37.3805P] 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_original_formula_sum        'C22.50 H28 Na O1.50 Pb'
_cod_database_code               7009950