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_7700991
_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         'C F3 O3 S, C31 H46 N3 O2, C3 H3'
_chemical_formula_sum            'C35 H49 F3 N3 O5 S'
_chemical_formula_weight         680.83
_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             2019-03-14
_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                 111.467(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.821(5)
_cell_length_b                   12.129(3)
_cell_length_c                   19.288(5)
_cell_measurement_reflns_used    3211
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      1.30
_cell_volume                     3662.2(17)
_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 1.000
_diffrn_measured_fraction_theta_max 0.979
_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  0.1385
_diffrn_reflns_av_unetI/netI     0.1619
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19822
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.619
_diffrn_reflns_theta_min         1.301
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0971 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.9283.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6767
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0941
_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^)+(0.1691P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2557
_refine_ls_wR_factor_ref         0.2904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3211
_reflns_number_total             6767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03099a2.cif
_cod_data_source_block           sh_0093m
_cod_depositor_comments
'Adding full bibliography for 7700989--7700996.cif.'
_cod_original_cell_volume        3662.3(18)
_cod_database_code               7700991
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F10A) \\sim Ueq, Uanis(F10B) \\sim Ueq, Uanis(F11A) \\sim Ueq,
Uanis(F11B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: F10A(0.5) F11A(0.5) F10B(0.5) F11B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C12(H12), C1(H1), C6(H6), C202(H202), C200(H200), C201(H201)
4.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C22(H22A,H22B,
 H22C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C23(H23A,
 H23B,H23C), C28(H28A,H28B,H28C), C61(H61A,H61B,H61C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'