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_4089433
_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         'C53 H61 N3 O Zr'
_chemical_formula_sum            'C53 H61 N3 O Zr'
_chemical_formula_weight         847.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2012-11-21
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372),
 SHELXL-2012,
 and manual edit
;
_cell_angle_alpha                70.279(3)
_cell_angle_beta                 81.233(3)
_cell_angle_gamma                74.687(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0034(6)
_cell_length_b                   13.0318(8)
_cell_length_c                   19.1179(13)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.27
_cell_volume                     2257.3(3)
_computing_cell_refinement       'SAINT V8.27B (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2011.2-3 (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 0.995
_diffrn_measured_fraction_theta_max 0.872
_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  0.0709
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            69838
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         31.081
_diffrn_reflns_theta_min         1.705
_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    0.284
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0837 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.8251.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.049
_refine_diff_density_min         -1.320
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.640
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         12640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.640
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0400P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9472
_reflns_number_total             12640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4001567_si_002.cif
_cod_data_source_block           compound7
_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               4089433
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H25 of C25, H21 of C21, H20 of C20, H19 of C19, H18 of C18, {H2A,H2B} of C2,
   H6 of C6, H8 of C8, {H1A,H1B} of C1, H52 of C52, H53 of C53, H27 of C27, H32
  of C32, {H33A,H33B} of C33, H35 of C35, H36 of C36, H37 of C37, H38 of C38,
  H39 of C39, {H40A,H40B} of C40, H42 of C42, H43 of C43, H44 of C44, H45 of
  C45, H46 of C46, {H47A,H47B} of C47, H49 of C49, H50 of C50, H51 of C51
 At 1.5 times of:
  {H16A,H16B,H16C} of C16, {H15A,H15B,H15C} of C15, {H10A,H10B,H10C} of C10,
  {H11A,H11B,H11C} of C11, {H12A,H12B,H12C} of C12, {H14A,H14B,H14C} of C14,
  {H29A,H29B,H29C} of C29, {H30A,H30B,H30C} of C30, {H31A,H31B,H31C} of C31
2.a Ternary CH refined with riding coordinates:
 C32(H32)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C33(H33A,H33B), C40(H40A,H40B), C47(H47A,H47B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C27(H27),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53)
2.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)
;
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.943
_shelx_hkl_checksum              93365
_shelx_res_checksum              73656
_shelxl_version_number           2012-6