Germylenes and stannylenes stabilized within N2PE rings (E = Ge or Sn): combined experimental and theoretical study.
Vrána, Jan; Ketkov, Sergey; Jambor, Roman; Růžička, Aleš; Lyčka, Antonín; Dostál, Libor; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10343–10354; doi:10.1039/c6dt01616b

data_7039313
_publ_section_title
;
 Germylenes and stannylenes stabilized within N2PE rings (E = Ge or Sn):
 combined experimental and theoretical study.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10343
_journal_page_last               10354
_journal_paper_doi               10.1039/c6dt01616b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C36 H63 Li2 N2 O2 P'
_chemical_formula_sum            'C36 H63 Li2 N2 O2 P'
_chemical_formula_weight         600.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-02 deposited with the CCDC.
2016-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3440(10)
_cell_length_b                   17.6920(15)
_cell_length_c                   10.6000(19)
_cell_measurement_reflns_used    3821
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      4.09
_cell_measurement_theta_min      26.39
_cell_volume                     3815.2(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26607
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         4.079
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.513
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.316
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3987
_refine_ls_number_restraints     255
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+3.4284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3041
_reflns_number_total             3987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01616b2.cif
_cod_data_source_block           5Et2O
_cod_depositor_comments
'Adding full bibliography for 7039310--7039320.cif.'
_cod_database_code               7039313
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C18 \\sim O2-C20 \\sim O2-C18A \\sim O2-C20A
 with sigma of 0.001
 C18-C19 \\sim C20-C21 \\sim C18A-C19A \\sim C20A-C21A
 with sigma of 0.001
 O2-C19 \\sim O2-C21 \\sim O2-C19A \\sim O2-C21A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C18A)
Uanis(C19) = Uanis(C19A)
Uanis(C20) = Uanis(C20A)
Uanis(C21) = Uanis(C21A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=
 Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=0.5*(1-
 FVAR(2))
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=
 Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=0.5*FVAR(2)
 Fixed Sof: H3A(0.5) H3B(0.5) H3C(0.5)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13)
6.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C18(H18A,H18B), C20(H20A,H20B), C18A(H18C,H18D), C20A(H20C,
 H20D)
6.c Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C19A(H19D,H19E,
 H19F), C21A(H21D,H21E,H21F)
6.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8)
6.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'