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_1556945
_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         'C40 H48 Br4 O4 Ti, 0.5(C8)'
_chemical_formula_sum            'C44 H48 Br4 O4 Ti'
_chemical_formula_weight         1008.35
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_Int_Tables_number      88
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.370(3)
_cell_length_b                   22.370(3)
_cell_length_c                   9.5963(14)
_cell_measurement_reflns_used    4264
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.76
_cell_measurement_theta_min      2.31
_cell_volume                     4802.2(11)
_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 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_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  0.0837
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19286
_diffrn_reflns_theta_full        25.6731
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         1.82
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.542
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1366 before and 0.0631 after correction. The Ratio of minimum to maximum transmission is 0.6367. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3947
_exptl_crystal_description       block
_exptl_crystal_F_000             2021.6064
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.163
_refine_diff_density_max         1.0492
_refine_diff_density_min         -0.5954
_refine_diff_density_rms         0.1415
_refine_ls_d_res_high            0.8203
_refine_ls_d_res_low             11.1849
_refine_ls_goodness_of_fit_ref   1.0431
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0431
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0557
_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^)+(0.1005P)^2^+9.6946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              27
_reflns_limit_h_min              0
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                1560
_reflns_number_total             2281
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9fd00033j2.cif
_cod_data_source_block           final
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        4802.0(12)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1556945
_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. Others
 Fixed Sof: C12(0.5) C11(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C2(H2)
3.b Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'