Kinetic stabilization of low-oxidation state and terminal hydrido main group metal complexes by a sterically demanding N,N'-bis(2,6-terphenyl)triazenide.
Leverett, Anthony R.; Diachenko, Vera; Cole, Marcus L.; McKay, Alasdair I.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13197–13204; doi:10.1039/c9dt02562f

data_7700750
_publ_section_title
;
 Kinetic stabilization of low-oxidation state and terminal hydrido main
 group metal complexes by a sterically demanding
 N,N'-bis(2,6-terphenyl)triazenide.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13197
_journal_page_last               13204
_journal_paper_doi               10.1039/c9dt02562f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C48 H51 Ge N3, 0.5(C7 H8)'
_chemical_formula_sum            'C51.5 H55 Ge N3'
_chemical_formula_weight         788.57
_chemical_name_common            '[GeH(N3Dmp2)]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-11 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                104.001(3)
_cell_angle_beta                 93.794(3)
_cell_angle_gamma                110.694(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4270(12)
_cell_length_b                   11.3856(13)
_cell_length_c                   20.013(2)
_cell_measurement_reflns_used    4924
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.102
_cell_measurement_theta_min      2.205
_cell_volume                     2126.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      149.9
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36335
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.422
_diffrn_reflns_theta_min         1.976
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0594 before and 0.0518 after correction. The Ratio of minimum to maximum transmission is 0.9208. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7829
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0689P)^2^+3.5398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4916
_reflns_number_total             7829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02562f2.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7700747--7700761.cif.'
_cod_original_cell_volume        2126.2(4)
_cod_original_formula_sum        'C51.50 H55 Ge N3'
_cod_database_code               7700750
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.942
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C49 \\sim C55: within 1.7A
with sigma of 0.03 and sigma for terminal atoms of 0.06
3. Rigid body (RIGU) restrains
 C55, C49, C54, C50, C53, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Ge1(0.5) Ge1A(0.5) C49(0.5) C54(0.5) H54(0.5) C53(0.5) H53(0.5)
 C52(0.5) H52(0.5) C51(0.5) H51(0.5) C50(0.5) H50(0.5) C55(0.5) H55A(0.5)
 H55B(0.5) H55C(0.5) H1A(0.5) H1(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4), C18(H18), C20(H20), C29(H29), C44(H44), C11(H11),
 C33(H33), C27(H27), C42(H42), C9(H9), C28(H28), C35(H35), C54(H54), C53(H53),
 C52(H52), C51(H51), C50(H50)
5.b Fitted hexagon refined as free rotating group:
 C49(C54,C53,C52,C51,C50)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C39(H39A,H39B,H39C), C24(H24A,H24B,H24C), C46(H46A,H46B,
 H46C), C37(H37A,H37B,H37C), C48(H48A,H48B,H48C), C14(H14A,H14B,H14C), C15(H15A,
 H15B,H15C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C47(H47A,H47B,H47C),
 C38(H38A,H38B,H38C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              39135
_olex2_submission_special_instructions 'No special instructions were received'