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_7707828
_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 ad
_chemical_formula_moiety         'C22 H27 N5 O4 Pd'
_chemical_formula_sum            'C22 H27 N5 O4 Pd'
_chemical_formula_weight         531.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-15 deposited with the CCDC.	2021-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.441(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.6646(5)
_cell_length_b                   12.2835(10)
_cell_length_c                   13.5762(10)
_cell_measurement_reflns_used    3839
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.744
_cell_measurement_theta_min      2.240
_cell_volume                     1106.40(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12875
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         1.507
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0469 before and 0.0436 after correction. The Ratio of minimum to maximum transmission is 0.7271. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_recrystallization_method
'Slow evaporation acetone:pentane solution (10:1) of compound.'
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 1953 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5069
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0277P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                4476
_reflns_number_total             5069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02531c2.cif
_cod_data_source_block           test4_c
_cod_depositor_comments
'Adding full bibliography for 7707825--7707829.cif.'
_cod_database_code               7707828
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.875
_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 Ternary CH refined with riding coordinates:
 C15(H15), C1(H1), C14(H14), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C7(H7), C8(H8)
2.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C20(H20A,H20B,
 H20C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              26138
_olex2_submission_original_sample_id KZ-1-58
_olex2_submission_special_instructions 'No special instructions were received'