Catalyst design insights from modelling a titanium-catalyzed multicomponent reaction.
Aldrich, Kelly E.; Kansal, Dhwani; Odom, Aaron L.; Faraday discussions 220 (2019) 208–230; doi:10.1039/c9fd00033j

data_1556944
_publ_section_title
;
 Catalyst design insights from modelling a titanium-catalyzed
 multicomponent reaction.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              208
_journal_page_last               230
_journal_paper_doi               10.1039/c9fd00033j
_journal_volume                  220
_journal_year                    2019
_chemical_formula_moiety
'0.67(C46 H60 O4 Ti), 0.5(C5 H11), 0.5(C5 H12)'
_chemical_formula_sum            'C35.67 H51.5 O2.67 Ti0.67'
_chemical_formula_weight         554.87
_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             2019-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-27 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.805(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   12.9534(4)
_cell_length_b                   21.2798(5)
_cell_length_c                   19.3799(4)
_cell_measurement_reflns_used    2667
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.04
_cell_measurement_theta_min      3.10
_cell_volume                     5279.0(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1608
_diffrn_reflns_av_unetI/netI     0.1946
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29158
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.441
_diffrn_reflns_theta_min         3.104
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0721 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.8878. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_description       cube
_exptl_crystal_F_000             1809
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         9480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.1797
_refine_ls_R_factor_gt           0.0791
_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^)+(0.0942P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1903
_refine_ls_wR_factor_ref         0.2350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3996
_reflns_number_total             9480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9fd00033j2.cif
_cod_data_source_block           p21_c_a
_cod_original_formula_sum        'C35.67 H51.50 O2.67 Ti0.67'
_cod_database_code               1556944
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.739
_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. Others
 Fixed Sof: C01G(0.75) H2AA(0.75) C01I(0.75) H3AA(0.75) HH(0.75) HI(0.75)
 C5(0.75) H5A(0.75) H5B(0.75) C7(0.75) H7A(0.75) H7B(0.75) H7C(0.75) C1(0.75)
 H1A(0.75) H1B(0.75) C2(0.75) H2A(0.75) H2B(0.75) H2C(0.75) C3(0.75) H3A(0.75)
 H3B(0.75) C4(0.75) H4A(0.75) H4B(0.75) C0AA(0.75) H0AB(0.75) H0AC(0.75)
 C1AA(0.75) H1AA(0.75) H1AB(0.75) H1AC(0.75)
3.a Secondary CH2 refined with riding coordinates:
 C00G(H00A,H00B), C00M(H00H,H00I), C5(H5A,H5B), C1(H1A,H1B), C3(H3A,H3B),
 C4(H4A,H4B), C0AA(H0AB,H0AC)
3.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00D(H00D), C00F(H00F), C00R(H00R), C00V(H00V), C00X(H00X),
 C00Z(H00Z), C013(H013), C01G(H2AA)
3.c Idealised Me refined as rotating group:
 C00L(H00C,H00E,H00G), C00P(H00J,H00K,H00L), C00Q(H00M,H00N,H00O), C00W(H00P,
 H00Q,H00S), C011(H01A,H01B,H01C), C012(H01D,H01E,H01F), C014(H01G,H01H,H01I),
 C017(H01J,H01K,H01L), C018(H01M,H01N,H01O), C019(H01P,H01Q,H01R), C01A(H01S,
 H01T,H01U), C01B(H01V,H01W,H01X), C01C(H01Y,H,HA), C01D(H01Z,HB,HC), C01E(H01,
 HD,HE), C01F(H0AA,HF,HG), C01I(H3AA,HH,HI), C7(H7A,H7B,H7C), C2(H2A,H2B,H2C),
 C1AA(H1AA,H1AB,H1AC)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'