Group 4 Transition-Metal Complexes of an Aniline‒Carbene‒Phenol Ligand
Despagnet-Ayoub, Emmanuelle; Henling, Lawrence M.; Labinger, Jay A.; Bercaw, John E.; Organometallics 32 (2013) 2934–; doi:10.1021/om4001567

data_4089431
_publ_section_title
;
 Group 4 Transition-Metal Complexes of an Aniline--Carbene--Phenol Ligand
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2934
_journal_paper_doi               10.1021/om4001567
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C36 H54 Cl3 N5 O Ti, 3(C H2 Cl2)'
_chemical_formula_sum            'C39 H60 Cl9 N5 O Ti'
_chemical_formula_weight         981.87
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2012-11-15
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372),
 SHELXL-2012,
 and manual edit
;
_cell_angle_alpha                90
_cell_angle_beta                 116.916(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5151(7)
_cell_length_b                   25.0837(13)
_cell_length_c                   15.3397(8)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.38
_cell_measurement_theta_min      2.73
_cell_volume                     4980.0(5)
_computing_cell_refinement       'SAINT V8.27B (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2012.2-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.27B (Bruker-AXS, 2007)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
 and SHELXTL (Bruker-AXS, 2007)
;
_computing_structure_refinement  'SHELXL-2012/6 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            158086
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         34.029
_diffrn_reflns_theta_min         1.624
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0607 before and 0.0540 after correction.
The Ratio of minimum to maximum transmission is 0.9268.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.689
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         19276
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.690
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0400P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13717
_reflns_number_total             19276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4001567_si_002.cif
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_source_target' value 'MO' was changed to 'Mo' in
accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4089431
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H39A,H39B} of C39, {H38A,H38B} of C38, H19 of C19, H20 of C20, H21 of C21,
  H25 of C25, H27 of C27, H32 of C32, H8 of C8, H6 of C6, {H2A,H2B} of C2, {H1A,
  H1B} of C1, H5 of N5, H3 of N3, H18 of C18, {H37B,H37A,H37D,H37C,H37F,H37E}
  of C37
 At 1.5 times of:
  {H29A,H29B,H29C} of C29, {H30A,H30B,H30C} of C30, {H31A,H31B,H31C} of C31,
  {H10A,H10B,H10C} of C10, {H11A,H11B,H11C} of C11, {H12A,H12B,H12C} of C12,
  {H14A,H14B,H14C} of C14, {H15A,H15B,H15C} of C15, {H16A,H16B,H16C} of C16,
  {H33A,H33B,H33C} of C33, {H34A,H34B,H34C} of C34, {H35A,H35B,H35C} of C35,
  {H36A,H36B,H36C} of C36
2. Others
 1*[Sof(Cl4A)+Sof(H37B)+Sof(H37A)]+1*[Sof(Cl4B)+Sof(H37D)+Sof(H37C)]+1*
 [Sof(Cl4C)+Sof(H37F)+Sof(H37E)]=1 with esd of 0.001
 Sof(Cl4A)=Sof(H37B)=Sof(H37A)
 Sof(Cl4B)=Sof(H37D)=Sof(H37C)
 Sof(Cl4C)=Sof(H37F)=Sof(H37E)
3.a Ternary CH refined with riding coordinates:
 N5(H5)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C37(H37B,H37A), C37(H37D,H37C), C37(H37F,H37E),
 C38(H38A,H38B), C39(H39A,H39B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C6(H6), C8(H8), C18(H18), C19(H19), C20(H20), C21(H21), C25(H25),
 C27(H27), C32(H32)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.810
_shelx_hkl_checksum              62475
_shelx_res_checksum              63374
_shelxl_version_number           2012-6