2,5-Di-(tert-butyl)phospholyl sandwich complexes containing group 14 elements (Ge, Sn, Pb). Synthesis, molecular structure, and ring transfer chemistry of [M(PC4H2But2)2] (M= Sn, Pb)
Forissier, Kareen; Ricard, Louis; Carmichael, Duncan; Mathey, François; Chemical Communications  (1999) 1273–; doi:10.1039/a902909e

data_7110555
_publ_section_title
;
 2,5-Di-(tert-butyl)phospholyl sandwich complexes containing group 14
 elements (Ge, Sn, Pb). Synthesis, molecular structure, and ring transfer
 chemistry of [M(PC4H2But2)2] (M= Sn, Pb)
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1273
_journal_paper_doi               10.1039/a902909e
_journal_year                    1999
_chemical_formula_sum            'C24 H40 P2 Sn'
_chemical_formula_weight         509.19
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.0890(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.0460(2)
_cell_length_b                   20.3280(2)
_cell_length_c                   16.3740(2)
_cell_measurement_reflns_used    545
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.0
_cell_volume                     5241.20(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10683
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         10683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+6.4407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                9926
_reflns_number_total             10683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902909Esup1.cif
_cod_data_source_block           snp2_2
_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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n        '
_cod_database_code               7110555