A new bis-phenolate mesoionic carbene ligand for early transition metal chemistry.
Baltrun, Marc; Watt, Fabian A.; Schoch, Roland; Wölper, Christoph; Neuba, Adam G.; Hohloch, Stephan; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14611–14625; doi:10.1039/c9dt03099a

data_7700995
_publ_section_title
;
 A new bis-phenolate mesoionic carbene ligand for early transition metal
 chemistry.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14611
_journal_page_last               14625
_journal_paper_doi               10.1039/c9dt03099a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C40 H57 N5 O2 Ti'
_chemical_formula_sum            'C40 H57 N5 O2 Ti'
_chemical_formula_weight         687.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-07 deposited with the CCDC.    2019-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.800(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.374(3)
_cell_length_b                   16.810(5)
_cell_length_c                   25.014(8)
_cell_measurement_reflns_used    4175
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.46
_cell_volume                     3941(2)
_computing_cell_refinement       'Bruker ApexIII suite, 2019'
_computing_data_collection       'Bruker ApexIII suite, 2019'
_computing_data_reduction        'Bruker ApexIII suite, 2019'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart AXS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_av_unetI/netI     0.0918
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26363
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.460
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.542117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1272 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.5421.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6902
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.0899
_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^)+(0.0851P)^2^+15.4015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2126
_refine_ls_wR_factor_ref         0.2468
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4175
_reflns_number_total             6902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03099a2.cif
_cod_data_source_block           sh_0167m
_cod_depositor_comments
'Adding full bibliography for 7700989--7700996.cif.'
_cod_database_code               7700995
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details   'Blessing, 1995'
_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. Shared sites
{N1, C2A}
{N1A, C2}
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uiso(N1) = Uiso(C2A)
Uiso(N1A) = Uiso(C2)
4. Others
 Sof(C61B)=Sof(H61D)=Sof(H61E)=Sof(H61F)=1-FVAR(1)
 Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(1)
 Fixed Sof: N1(0.5) C2A(0.5) C2(0.5) N1A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C14(H14), C104(H104), C12(H12), C100(H100), C103(H103),
 C102(H102), C101(H101)
5.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C31(H31A,H31B,
 H31C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C61A(H61A,H61B,H61C), C61B(H61D,H61E,
 H61F), C42(H42A,H42B,H42C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'