Oxidative addition to M(II) (M = Ge, Sn) amidinate complexes: routes to group 14 chalcogenolates with hypervalent coordination environments
Foley, Stephen R.; Yap, Glenn P. A.; Richeson, Darrin S.; Journal of the Chemical Society, Dalton Transactions  (2000) 1663–; doi:10.1039/a909228e

data_7009194
_publ_section_title
;
 Oxidative addition to M(II) (M&#x2005;=&#x2005;Ge, Sn) amidinate
 complexes: routes to group 14 chalcogenolates with hypervalent
 coordination environments
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1663
_journal_paper_doi               10.1039/a909228e
_journal_year                    2000
_chemical_formula_sum            'C40 H60 Ge N4 Se2'
_chemical_formula_weight         827.43
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.72(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.953(2)
_cell_length_b                   19.181(4)
_cell_length_c                   18.909(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     3959.1(14)
_computing_cell_refinement       'Rigaku AFC6S'
_computing_data_collection       'Rigaku AFC6S'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3879
_diffrn_reflns_theta_full        20.70
_diffrn_reflns_theta_max         20.70
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    2.645
_exptl_absorpt_correction_T_max  0.98253
_exptl_absorpt_correction_T_min  0.25631
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi-scans method by North'
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         3879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1254P)^2^+34.1127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.1997
_reflns_number_gt                3490
_reflns_number_total             3879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909228e.txt
_cod_data_source_block           dr135
_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 
;
_cod_original_cell_volume        3959(1)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009194