Polyannulated Bis(N-heterocyclic carbene)palladium Pincer Complexes for Electrocatalytic CO2 Reduction.
Therrien, Jeffrey A.; Wolf, Michael O.; Patrick, Brian O.; Inorganic chemistry 54 (2015) 11721–11732; doi:10.1021/acs.inorgchem.5b01698

data_4346571
_publ_section_title
;
 Polyannulated Bis(N-heterocyclic carbene)palladium Pincer Complexes for
 Electrocatalytic CO2 Reduction.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11721
_journal_page_last               11732
_journal_paper_doi               10.1021/acs.inorgchem.5b01698
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C45 H41 Cl N5 Pd, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C48 H44 Cl F3 N6 O3 Pd S'
_chemical_formula_weight         983.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 130.0121(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.8478(13)
_cell_length_b                   9.8610(5)
_cell_length_c                   20.2588(10)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      2.28
_cell_volume                     4260.9(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.099
_diffrn_reflns_theta_min         1.910
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0559 before and 0.0486 after correction.
 The Ratio of minimum to maximum transmission is 0.89.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0610 before and 0.0494 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 65576 reflections, Rint = 0.0435
 (47327 with I > 3sig(I), Rint = 0.0397)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 5451 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.188(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         20995
_refine_ls_number_restraints     556
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0410P)^2^+1.7078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                19678
_reflns_number_total             20995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01698_si_002.cif
_cod_data_source_block           mw260
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/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 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4346571
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.25(3) 0.245(17) 0.259(14) 0.245(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C43-C44 \\sim C43-C44A
 with sigma of 0.01
 C44-C45 \\sim C44A-C45A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C44A) = Uanis(C44)
Uanis(C45) = Uanis(C45A)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45D)=
 Sof(H45E)=Sof(H45F)=1-FVAR(1)
 Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C22(H22A,H22B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,
 H40B), C42(H42A,H42B), C43(H43A,H43B), C43(H43C,H43D), C44(H44A,H44B),
 C44A(H44C,H44D)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C18(H18), C19(H19), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33), C34(H34)
7.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C45A(H45D,H45E,
 H45F)
;
_shelx_res_checksum              6741
_shelx_hkl_checksum              69914
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'