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

data_7039317
_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         'C30 H50 Li N4 P'
_chemical_formula_sum            'C30 H50 Li N4 P'
_chemical_formula_weight         504.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-09
_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                 107.28(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.463(2)
_cell_length_b                   24.322(5)
_cell_length_c                   13.238(3)
_cell_measurement_reflns_used    12994
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     3216.8(13)
_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      150.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_min         2.204
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_min  0.628414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1246 before and 0.0316 after correction.
The Ratio of minimum to maximum transmission is 0.6284.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   0.756
_exptl_transmission_factor_min   0.475
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3671
_refine_ls_number_restraints     334
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+3.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2402
_reflns_number_total             3671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01616b2.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 7039310--7039320.cif.'
_cod_original_cell_volume        3216.7(12)
_cod_database_code               7039317
_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
 N2-C21 \\sim N2-C22 \\sim N3-C31 \\sim N3-C32
 with sigma of 0.02
 N2-C23 \\sim N3-C33
 with sigma of 0.02
 C21-C22 \\sim C31-C32
 with sigma of 0.02
 C21-C23 \\sim C22-C23 \\sim C31-C33 \\sim C32-C33
 with sigma of 0.02
 N2-C33 \\sim N3-C23
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1A) = Uanis(C1B)
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C3B)
Uanis(C4A) = Uanis(C4B)
Uanis(C5A) = Uanis(C5B)
Uanis(C6A) = Uanis(C6B)
Uanis(C7A) = Uanis(C7B)
Uanis(C8A) = Uanis(C8B)
Uanis(C9A) = Uanis(C9B)
Uanis(C10A) = Uanis(C10B)
Uanis(C11A) = Uanis(C11B)
Uanis(C12A) = Uanis(C12B)
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. Same fragment restrains
{C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B, C11B, C12B} sigma for 1-2:
0.01, 1-3: 0.04
as
{C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A}
6. Others
 Sof(C1B)=Sof(C2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=
 Sof(C6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=
 Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: N2(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C23(0.5) H23A(0.5) H23B(0.5) N3(0.5) C31(0.5) H31A(0.5)
 H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C33(0.5) H33A(0.5)
 H33B(0.5)
7.a Ternary CH refined with riding coordinates:
 C7A(H7A), C10A(H10A), C7B(H7B), C10B(H10B)
7.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C33(H33A,H33B)
7.c Me refined with riding coordinates:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C11A(H11A,H11B,H11C), C12A(H12A,
 H12B,H12C), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C11B(H11D,H11E,H11F),
 C12B(H12D,H12E,H12F)
7.d Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C5A(H5A), C3B(H3B), C4B(H4B), C5B(H5B)
7.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C)
;
_shelx_shelxl_version_number     2014/7