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_1556947
_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         'C44 H60 O4 Ti, 0.75(C6 H14)'
_chemical_formula_sum            'C48.5 H70.5 O4 Ti'
_chemical_formula_weight         765.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-03 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.452(2)
_cell_length_b                   9.4744(8)
_cell_length_c                   22.253(2)
_cell_measurement_reflns_used    6652
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.33
_cell_volume                     4733.3(7)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18717
_diffrn_reflns_theta_full        25.4042
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.81
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0715 before and 0.0478 after correction. The Ratio of minimum to maximum transmission is 0.9168. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.0741
_exptl_crystal_description       plate
_exptl_crystal_F_000             1663.8352
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.402
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.6453
_refine_diff_density_min         -0.3466
_refine_diff_density_rms         0.0673
_refine_ls_d_res_high            0.8284
_refine_ls_d_res_low             11.2249
_refine_ls_goodness_of_fit_ref   1.0323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4367
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0322
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1292P)^2^+1.8643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1958
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              -26
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                3350
_reflns_number_total             4367
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9fd00033j2.cif
_cod_data_source_block           DK_III_13feb2018_1
_cod_database_code               1556947
_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. Restrained distances
 C24-C25
 1.55 with sigma of 0.02
3. Others
 Fixed Sof: C24(0.75) H24a(0.75) H24b(0.75) C23(0.75) H23b(0.75) H23a(0.75)
 C25(0.75) H25a(0.75) H25b(0.75) H25c(0.75)
4.a Riding coordinates:
 C25(H25a,H25b,H25c)
4.b Secondary CH2 refined with riding coordinates:
 C24(H24a,H24b), C23(H23a,H23b)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C16(H16), C3(H3), C13(H13), C14(H14), C5(H5)
4.d Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C10(H10a,H10b,H10c), C9(H9a,H9b,H9c), C20(H20a,H20b,
 H20c), C11(H11a,H11b,H11c), C22(H22a,H22b,H22c), C18(H18a,H18b,H18c), C7(H7a,
 H7b,H7c)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'