Azametallatranes of Group 14 Elements. Syntheses and X-ray Studies
Shutov, Pavel L.; Sorokin, Denis A.; Karlov, Sergey S.; Harms, Klaus; Oprunenko, Yuri F.; Churakov, Andrei V.; Antipin, Mikhail Yu.; Zaitseva, Galina S.; Lorberth, Jörg; Organometallics 22 (2003) 516–522; doi:10.1021/om020708h

data_4060714
_publ_section_title
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 Azametallatranes of Group 14 Elements. Syntheses and X-ray Studies
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_journal_coden_ASTM              ORGND7
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              516
_journal_page_last               522
_journal_paper_doi               10.1021/om020708h
_journal_volume                  22
_journal_year                    2003
_chemical_formula_sum            'C15 H26 Ge N4'
_chemical_formula_weight         334.99
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3466(6)
_cell_length_b                   11.2962(8)
_cell_length_c                   16.3629(11)
_cell_measurement_reflns_used    3784
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.19
_cell_volume                     1542.8(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_method       \w
_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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11023
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.983
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4298
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.193
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.049
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_restrained_S_obs      1.049
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_obs          0.0383
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0956
_refine_ls_wR_factor_obs         0.0945
_reflns_number_observed          3198
_reflns_number_total             3369
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            om020708h.cif
_cod_data_source_block           z
_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^)+(0.0673P)^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^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 4609 2016-04-01 06:22:49Z antanas 
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_cod_database_code               4060714