Structural diversity in a homologous series of donor free alkali metal complexes bearing a sterically demanding triazenide.
McKay, Alasdair I.; Cole, Marcus L.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2948–2952; doi:10.1039/c8dt04983a

data_7048897
_publ_section_title
;
 Structural diversity in a homologous series of donor free alkali metal
 complexes bearing a sterically demanding triazenide.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2948
_journal_page_last               2952
_journal_paper_doi               10.1039/c8dt04983a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C56 H66 Li N3 O2, C4 H8 O'
_chemical_formula_sum            'C60 H74 Li N3 O3'
_chemical_formula_weight         892.16
_chemical_name_common            '[Li(N3Dmp2)(OC4H8)2].OC4H8'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-19 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.2130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9250(4)
_cell_length_b                   17.6801(5)
_cell_length_c                   24.5702(7)
_cell_measurement_reflns_used    7079
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.165
_cell_measurement_theta_min      2.451
_cell_volume                     5139.3(3)
_computing_cell_refinement       'SAINT V8.30C (?, 2016)'
_computing_data_reduction        'SAINT V8.30C (?, 2016)'
_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(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40773
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.114
_diffrn_reflns_theta_min         2.522
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0596 before and 0.0548 after correction. The Ratio of minimum to maximum transmission is 0.9131. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       prism
_exptl_crystal_F_000             1928
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         11155
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0786P)^2^+1.3204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7361
_reflns_number_total             11155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04983a2.cif
_cod_data_source_block           data7
_cod_depositor_comments
'Adding full bibliography for 7048890--7048897.cif.'
_cod_database_code               7048897
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.986
_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-C53 \\sim O2-C56
 with sigma of 0.02
 O2A-C53A \\sim O2A-C56A
 with sigma of 0.02
 C54-C56 \\sim C53-C55
 with sigma of 0.04
 C54A-C56A \\sim C53A-C55A
 with sigma of 0.04
 O2-C54 \\sim O2-C55
 with sigma of 0.04
 O2A-C54A \\sim O2A-C55A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O2A \\sim C53A \\sim C54A \\sim C55A \\sim C56A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O2, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2A, C53A, C54A, C55A, C56A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O2A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C54A)=Sof(H54C)=Sof(H54D)=
 Sof(C55A)=Sof(H55C)=Sof(H55D)=Sof(C56A)=Sof(H56C)=Sof(H56D)=1-FVAR(1)
 Sof(O2)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=
 Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C60(H60A,
 H60B), C59(H59A,H59B), C58(H58A,H58B), C57(H57A,H57B), C53(H53A,H53B),
 C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C53A(H53C,H53D), C54A(H54C,
 H54D), C55A(H55C,H55D), C56A(H56C,H56D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C18(H18), C20(H20), C27(H27),
 C28(H28), C29(H29), C33(H33), C35(H35), C42(H42), C44(H44)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              98018
_olex2_exptl_crystal_mounting_method
'MiTeGen microloop in type NVH immersion oil'
_olex2_submission_special_instructions 'No special instructions were received'