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_7700994
_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 Cl N5 Nb O2, C4 H10 O'
_chemical_formula_sum            'C44 H67 Cl N5 Nb O3'
_chemical_formula_weight         842.38
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-04
_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                103.559(3)
_cell_angle_beta                 93.800(3)
_cell_angle_gamma                108.092(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0086(16)
_cell_length_b                   15.840(2)
_cell_length_c                   15.982(2)
_cell_measurement_reflns_used    7628
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.53
_cell_measurement_theta_min      1.32
_cell_volume                     2545.9(6)
_computing_cell_refinement       'Bruker Apex3 software, 2019'
_computing_data_collection       'Bruker Apex3 software, 2019'
_computing_data_reduction        'Bruker Apex3 software, 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 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29018
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.538
_diffrn_reflns_theta_min         1.326
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1171 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.8190.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.074
_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     536
_refine_ls_number_reflns         9465
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+1.9857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7628
_reflns_number_total             9465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03099a2.cif
_cod_data_source_block           sh_0198_0m
_cod_depositor_comments
'Adding full bibliography for 7700989--7700996.cif.'
_cod_original_cell_volume        2545.9(7)
_cod_database_code               7700994
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C102(H10D,H10E), C101(H10I,H10J)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C12(H12), C53(H53), C14(H14), C54(H54), C50(H50), C52(H52),
 C51(H51)
4.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C19(H19A,H19B,H19C), C24(H24A,H24B,H24C), C61(H61A,H61B,
 H61C), C32(H32A,H32B,H32C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C22(H22A,
 H22B,H22C), C43(H43A,H43B,H43C), C41(H41A,H41B,H41C), C18(H18A,H18B,H18C),
 C30(H30A,H30B,H30C), C20(H20A,H20B,H20C), C103(H10A,H10B,H10C), C100(H10F,H10G,
 H10H), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C),
 C28A(H28D,H28E,H28F), C27A(H27D,H27E,H27F), C26A(H26D,H26E,H26F)
;
_olex2_submission_special_instructions 'No special instructions were received'