Synthesis, Cycloaddition, and Cycloreversion Reactions of Mononuclear Titanocene–oxo Complexes
Nguyen, Trang T.; Kortman, Gregory D.; Hull, Kami L.; Organometallics 35 (2016) 1713–; doi:10.1021/acs.organomet.6b00111

data_4086503
_publ_contact_author
; 
Kami L. Hull
University of Illinois 
361 RAL, Box 23-5
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Synthesis, Cycloaddition, and Cycloreversion Reactions of Mononuclear
 Titanocene--oxo Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1713
_journal_paper_doi               10.1021/acs.organomet.6b00111
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C100 H140 N4 O4 Ti4'
_chemical_formula_weight         1653.75
_chemical_name_systematic
; 
C25 H35 N O Ti 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2b'
_space_group_name_H-M_alt        'P b c 21'
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-22
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1911(4)
_cell_length_b                   16.9206(4)
_cell_length_c                   17.1163(4)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.68
_cell_volume                     4399.62(19)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
; 
SHELX-2014-6 (Sheldrick, 2014) 
Olex2 1.2.6 (Dolomanov et. al., 2009) 
;
_computing_structure_solution    'SHELX-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm92p_0m
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13309
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.566
_diffrn_reflns_theta_min         1.340
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.2901
_exptl_absorpt_correction_T_min  0.1880
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_id                cm92p_0m
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 -4 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.468
_exptl_crystal_size_mid          0.414
_exptl_crystal_size_min          0.297
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         13309
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0710P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                11473
_reflns_number_total             13309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00111_si_002.cif
_cod_data_source_block           cm92p_0m
_cod_depositor_comments
'Adding full bibliography for 4086503--4086505.cif.'
_cod_database_code               4086503
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.833
_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.a Aromatic/amide H refined with riding coordinates: 
 C14A(H14A), C5A(H5A), C5(H), C19(HA), C19A(H19A), C21(HE), C21A(H21A), 
 C23A(H23A), C23(H0AA), C14(H1BA) 
2.b Idealised Me refined as rotating group: 
 C6A(H6AA,H6AB,H6AC), C17(HB,HC,HD), C15A(H15A,H15B,H15C), C17A(H17A,H17B, 
 H17C), C25(HF,HG,HH), C7A(H7AA,H7AB,H7AC), C9A(H9AA,H9AB,H9AC), C8A(H8AA,H8AB, 
 H8AC), C24A(H24A,H24B,H24C), C15(HI,HJ,HK), C16A(H16A,H16B,H16C), C7(HL,HM,HN), 
  C25A(H25A,H25B,H25C), C16(HO,HP,HQ), C8(HR,HS,HT), C6(HU,HV,HW), C9(HX,HY,HZ), 
  C24(H1AA,H2AA,H3AA), C18(H4AA,H5AA,H0BA), C18A(H18A,H18B,H18C) 
;
_shelx_res_checksum              84552
_shelx_hkl_checksum              53192
_olex2_submission_special_instructions 'No special instructions were received'