Preparation, characterization and reactivity of trifluoromethoxy palladium(ii) complexes
Xu, Songsong; Shao, Yingbo; Zheng, Hanliang; Leng, Xuebing; Xue, Xiao-Song; Shen, Qilong; New Journal of Chemistry 46 (2022) 20760–20767; doi:10.1039/D2NJ04198G

data_7061944
_publ_section_title
;
 Preparation, characterization and reactivity of trifluoromethoxy
 palladium(ii) complexes
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20760
_journal_page_last               20767
_journal_paper_doi               10.1039/D2NJ04198G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C14 H20 F6 N2 O Pd'
_chemical_formula_sum            'C14 H20 F6 N2 O Pd'
_chemical_formula_weight         452.72
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-09-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-25 deposited with the CCDC.	2022-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   22.1489(5)
_cell_length_b                   22.1489(5)
_cell_length_c                   14.1421(3)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      54.930
_cell_measurement_theta_min      5.021
_cell_volume                     6937.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.995
_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  0.0249
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16497
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         2.510
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1525 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3401
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+3.1678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0420
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3296
_reflns_number_total             3401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04198g2.cif
_cod_data_source_block           mo_d8v191192_0m
_cod_depositor_comments
'Adding full bibliography for 7061942--7061946.cif.'
_cod_database_code               7061944
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.822
_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
 C1-C2 = C1'-C2'
 1.55 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C1' \\sim C2': within 2A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 2A
Uanis(F1') \\sim Ueq, Uanis(F2') \\sim Ueq, Uanis(F3') \\sim Ueq, Uanis(F4')
\\sim Ueq, Uanis(F5') \\sim Ueq, Uanis(F6') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C1(0.7) H1A(0.7) H1B(0.7) C2(0.7) H2A(0.7) H2B(0.7) C1'(0.3)
 H1'A(0.3) H1'B(0.3) C2'(0.3) H2'A(0.3) H2'B(0.3) F1(0.5) F2(0.5) F3(0.5)
 F4(0.5) F5(0.5) F6(0.5) F1'(0.5) F2'(0.5) F3'(0.5) F4'(0.5) F5'(0.5) F6'(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C1'(H1'A,H1'B), C2'(H2'A,H2'B)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              20367
_olex2_submission_special_instructions 'No special instructions were received'