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_1556950
_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 H48 F12 O4 Ti'
_chemical_formula_sum            'C44 H48 F12 O4 Ti'
_chemical_formula_weight         916.72
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-02
_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                 110.609(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0590(7)
_cell_length_b                   9.8711(3)
_cell_length_c                   22.6307(6)
_cell_measurement_reflns_used    4843
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.62
_cell_measurement_theta_min      4.17
_cell_volume                     4612.4(2)
_computing_cell_refinement       'APEX2 (BRUKER, V2012.10-0, 2012)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.946
_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  0.0713
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14837
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.047
_diffrn_reflns_theta_min         4.174
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.348
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.5798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1313 before and 0.0626 after correction. The Ratio of minimum to maximum transmission is 0.7695. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       needle
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.603
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0885
_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^)+(0.1677P)^2^+12.3775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2590
_refine_ls_wR_factor_ref         0.2860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3234
_reflns_number_total             4284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9fd00033j2.cif
_cod_data_source_block           dk_4august_final
_cod_database_code               1556950
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.332
_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. Uiso/Uaniso restraints and constraints
Uanis(F6B) = Uanis(F6A) = Uanis(F4B) = Uanis(F4A) = Uanis(F5B) = Uanis(F5A) =
Uanis(F3A) = Uanis(F3B) = Uanis(F1A) = Uanis(F1B) = Uanis(F2A) = Uanis(F2B)
3. Others
 Fixed Sof: F2A(0.5) F1A(0.5) F3A(0.5) F4B(0.5) F5B(0.5) F6B(0.5) F1B(0.5)
 F3B(0.5) F2B(0.5) F4A(0.5) F6A(0.5) F5A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3), C16(H16), C17(H17), C14(H14)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C),
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'