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_1556948
_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         'C29 H44 O4 Ti, C H Cl3'
_chemical_formula_sum            'C30 H45 Cl3 O4 Ti'
_chemical_formula_weight         623.91
_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             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                67.6580(10)
_cell_angle_beta                 80.5460(10)
_cell_angle_gamma                66.6990(10)
_cell_formula_units_Z            2
_cell_length_a                   11.57250(10)
_cell_length_b                   12.38990(10)
_cell_length_c                   13.0612(2)
_cell_measurement_reflns_used    5635
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.02
_cell_measurement_theta_min      3.66
_cell_volume                     1590.67(3)
_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      173.01
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20754
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.176
_diffrn_reflns_theta_min         3.659
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.849
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0790 before and 0.0592 after correction. The Ratio of minimum to maximum transmission is 0.7854. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5629
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0844P)^2^+0.1693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4246
_reflns_number_total             5629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9fd00033j2.cif
_cod_data_source_block           rjs
_cod_database_code               1556948
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.625
_shelx_estimated_absorpt_t_min   0.429
_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
 C1-C2 \\sim C011-C010 \\sim C1-C0 \\sim C012-C011
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C012) = Uanis(C0)
Uanis(C010) = Uanis(C2)
Uanis(C011) = Uanis(C1)
4. Others
 Sof(C1)=Sof(H1)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(H0C)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(H2C)=1-FVAR(1)
 Sof(C010)=Sof(H01A)=Sof(H01B)=Sof(H01C)=Sof(C011)=Sof(H011)=Sof(C012)=
 Sof(H01D)=Sof(H01E)=Sof(H01F)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C00O(H00O), C00Z(H2AA), C011(H011), C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C00J(H00A,H00C)
5.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00E(H00E), C00G(H00G), C00N(H00N)
5.d Idealised Me refined as rotating group:
 C00P(H00D,H00F,H00H), C00Q(H00I,H00J,H00K), C00R(H00L,H00M,H00P), C00S(H00Q,
 H00R,H00S), C00T(H00T,H00U,H00V), C00U(H00W,H00X,H00Y), C00V(H00Z,H,HA),
 C00W(H00,HB,HC), C00X(H0AA,HD,HE), C00Y(H1AA,HF,HG), C010(H01A,H01B,H01C),
 C012(H01D,H01E,H01F), C0(H0A,H0B,H0C), C2(H2A,H2B,H2C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'