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_1556952
_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         'C23 H30 I2 O2 Ti'
_chemical_formula_sum            'C23 H30 I2 O2 Ti'
_chemical_formula_weight         640.17
_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                90.518(7)
_cell_angle_beta                 92.411(5)
_cell_angle_gamma                95.161(4)
_cell_formula_units_Z            2
_cell_length_a                   9.6900(10)
_cell_length_b                   9.8844(13)
_cell_length_c                   13.151(2)
_cell_measurement_reflns_used    720
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.07
_cell_measurement_theta_min      25.12
_cell_volume                     1253.3(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      173.0
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.964
_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  0.1065
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15520
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.154
_diffrn_reflns_theta_min         4.492
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.340
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.4177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1246 before and 0.0743 after correction. The Ratio of minimum to maximum transmission is 0.5547. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.185
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0596P)^2^+0.9570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3281
_reflns_number_total             4410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9fd00033j2.cif
_cod_data_source_block           early_a
_cod_database_code               1556952
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.329
_shelx_estimated_absorpt_t_min   0.123
_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.a Secondary CH2 refined with riding coordinates:
 C00G(H00E,H00G)
2.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00F(H00F), C00O(H00T), C00Q(H00X)
2.c Idealised Me refined as rotating group:
 C00E(H00B,H00C,H00D), C00I(H00H,H00I,H00J), C00L(H00K,H00L,H00M), C00M(H00N,
 H00O,H00P), C00N(H00Q,H00R,H00S), C00P(H00U,H00V,H00W), C00R(H00Y,H,HA),
 C00S(H00Z,HB,HC)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'