Chiral tridentate bis(oxazol-2-ylimino) isoindoline-based pincer ligands: isolation and characterization <i>via</i> deligation from <i>in situ</i> prepared Cd-ligand complexes.
Zivkovic, Kristina; Baldauf, Lilia M.; Cryder, Jessica L.; Villaseñor, Alexa; Reyes, Valeria; Bernier, Lauren E.; Thomas, Theresa J.; O'Toole, Maxwell; Fulton, Kayleen; Moore, Curtis E.; Rheingold, Arnold L.; Daley, Christopher J. A.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10041–10049; doi:10.1039/d0dt02531c

data_7707827
_publ_section_title
;
 Chiral tridentate bis(oxazol-2-ylimino) isoindoline-based pincer ligands:
 isolation and characterization <i>via</i> deligation from <i>in situ</i>
 prepared Cd-ligand complexes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10041
_journal_page_last               10049
_journal_paper_doi               10.1039/d0dt02531c
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C20 H25 N5 O2'
_chemical_formula_sum            'C20 H25 N5 O2'
_chemical_formula_weight         367.45
_chemical_name_systematic
1,3-bis(4,5-dihydro-4-(S)-iso-propyloxazol-2-ylimino)isoindoline
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-13 deposited with the CCDC.	2021-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                100.313(2)
_cell_angle_beta                 109.063(2)
_cell_angle_gamma                110.537(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2785(4)
_cell_length_b                   10.8229(4)
_cell_length_c                   11.2472(4)
_cell_measurement_reflns_used    7586
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.45
_cell_measurement_theta_min      4.41
_cell_volume                     943.06(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.934
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10393
_diffrn_reflns_point_group_measured_fraction_full 0.712
_diffrn_reflns_point_group_measured_fraction_max 0.706
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.099
_diffrn_reflns_theta_min         4.409
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.151
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 1464 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.21(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         4863
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0361P)^2^+0.1916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.512
_reflns_Friedel_fraction_full    0.483
_reflns_Friedel_fraction_max     0.478
_reflns_number_gt                4596
_reflns_number_total             4863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02531c2.cif
_cod_data_source_block           daley13
_cod_depositor_comments
'Adding full bibliography for 7707825--7707829.cif.'
_cod_database_code               7707827
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.891
_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
 N3-H3 = N3'-H3'
 0.9 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C3(H3A), C4(H4), C17(H17), C18(H18), C3'(H3'A), C4'(H4'), C17'(H17'),
 C18'(H18')
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C16(H16A,H16B), C5'(H5'A,H5'B), C16'(H16C,H16D)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C9'(H9'), C10'(H10'), C11'(H11'),
 C12'(H12')
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C1'(H1'A,H1'B,H1'C), C2'(H2'A,H2'B,H2'C), C19'(H19D,H19E,H19F), C20'(H20D,H20E,
 H20F)
;
_shelx_res_checksum              4814
_olex2_submission_special_instructions 'No special instructions were received'