Novel germanium(ii) binaphthoxide complexes: synthesis and crystal structure of (R,R)-[Ge{OC20H10(OSiMe3)-2'-(SiMe3)2-3,3'}2] and (R)-[Ge{O2C20H10(SiMe2Ph)2-3,3'}{NH3}]; catalytic function of Ge[N(SiMe3)2]2 for the mono-silylation of 3,3'-disubstituted-1,1'-bi-2,2'-naphthols
Weinert, Charles S.; Fanwick, Phillip E.; Rothwell, Ian P.; Journal of the Chemical Society, Dalton Transactions  (2002) 2948–; doi:10.1039/b204299a

data_7011818
_publ_section_title
;
 Novel germanium(ii) binaphthoxide complexes: synthesis and crystal
 structure of (R,R)-[Ge{OC20H10(OSiMe3)-2'-(SiMe3)2-3,3'}2] and
 (R)-[Ge{O2C20H10(SiMe2Ph)2-3,3'}{NH3}]; catalytic function of
 Ge[N(SiMe3)2]2 for the mono-silylation of
 3,3'-disubstituted-1,1'-bi-2,2'-naphthols
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2948
_journal_paper_doi               10.1039/b204299a
_journal_year                    2002
_chemical_formula_moiety         'C36 H35 Ge1 N1 O2 Si2'
_chemical_formula_sum            'C36 H35 Ge N O2 Si2'
_chemical_formula_weight         642.45
_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_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             13-11-01
_audit_creation_method           from_MolEN_and_SHELXL
_audit_update_record             ' ?'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3277(2)
_cell_length_b                   10.4652(3)
_cell_length_c                   36.0635(8)
_cell_measurement_reflns_used    20161
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3142.97(14)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
;
ORTEP (Johnson, 1976)
PLUTON (Spek, 1991)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    PATTY_(DIRDIF99,_Beurskins,_1999)
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.9889
_diffrn_measured_fraction_theta_max 0.9889
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            20161
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         5.00
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  0.8988
_exptl_absorpt_correction_T_min  0.5423
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.47
_refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment
;
Chemically significant hydrogens refined isotropically
Others riding
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6841
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3  '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.077
_reflns_number_gt                5769
_reflns_number_total             6841
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            b204299a.txt
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_geom_angle_publ_flag'
value 'YES' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (79
times).

'_geom_bond_publ_flag' value 'YES' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (51 time).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3143.0(2)
_cod_original_formula_sum        'C36 H35 Ge1 N1 O2 Si2'
_cod_database_code               7011818
_reflns_friedl_coverage          0.8250