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_1556951
_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         'C62 H81 N3 O4 Ti2, 0.5(C6 H14)'
_chemical_formula_sum            'C65 H88 N3 O4 Ti2'
_chemical_formula_weight         1071.18
_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             2019-03-25
_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
_cell_angle_beta                 121.054(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.0256(18)
_cell_length_b                   17.3283(7)
_cell_length_c                   25.5196(12)
_cell_measurement_reflns_used    9449
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.21
_cell_measurement_theta_min      2.97
_cell_volume                     12890.1(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_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  0.1037
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            83762
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         2.967
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.448
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 172391 reflections, Rint = 0.1500
 (19148 with I > 3sig(I), Rint = 0.0549)
;
_exptl_crystal_colour            'orangish brown'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       block
_exptl_crystal_F_000             4600
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         11768
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0983P)^2^+14.4446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8329
_reflns_number_total             11768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9fd00033j2.cif
_cod_data_source_block           c2c_early_a
_cod_database_code               1556951
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.695
_shelx_estimated_absorpt_t_min   0.611
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1S-C3S = C2S-C4S = C3S-C5S = C4S-C6S
 2.2 with sigma of 0.002
 C1S-C2S \\sim C3S-C2S \\sim C3S-C4S \\sim C5S-C4S \\sim C6S-C5S
 with sigma of 0.02
3. Others
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) C5S(0.5)
 H5SA(0.5) H5SB(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5)
4.a Ternary CH refined with riding coordinates:
 N007(H007)
4.b Secondary CH2 refined with riding coordinates:
 C00M(H00A,H00B), C00N(H00C,H00D), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,
 H4SB), C5S(H5SA,H5SB)
4.c Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00K(H00K), C00L(H00L), C00Q(H00Q), C00S(H00S), C00T(H00T),
 C01B(H01B), C01E(H01H), C01G(H01L), C01P(H01), C012(H012), C013(H013),
 C014(H014), C016(H016), C018(H018), C019(H019)
4.d Idealised Me refined as rotating group:
 C00V(H00F,H00G,H00H), C01C(H01A,H01C,H01D), C01D(H01E,H01F,H01G), C01F(H01I,
 H01J,H01K), C01H(H01M,H01N,H01O), C01I(H01P,H01Q,H01R), C01J(H01S,H01T,H01U),
 C01K(H01V,H01W,H01X), C01M(H01Y,H,HA), C01O(H01Z,HB,HC), C01Q(H0AA,HD,HE),
 C01R(H1AA,HF,HG), C01S(H2AA,HH,HI), C01T(H3AA,HJ,HK), C01U(H4AA,HL,HM),
 C01V(H5AA,HN,HO), C01W(H6AA,HP,HQ), C01X(H7AA,HR,HS), C01Y(H8AA,HT,HU),
 C01Z(H9AA,HV,HW), C1S(H1SA,H1SB,H1SC), C6S(H6SA,H6SB,H6SC)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'