Synthesis, structural characterization, and coordination chemistry of imidazole-based alkylidene ketenes.
Feuerstein, Wolfram; Varava, Paul; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Severin, Kay; Chemical communications (Cambridge, England) 57 (2021) 11509–11512; doi:10.1039/d1cc05161j

data_7129125
_publ_section_title
;
 Synthesis, structural characterization, and coordination chemistry of
 imidazole-based alkylidene ketenes.
;
_journal_issue                   87
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11509
_journal_page_last               11512
_journal_paper_doi               10.1039/d1cc05161j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C32 H41 Cl N2 O Pd, C6 H6'
_chemical_formula_sum            'C38 H47 Cl N2 O Pd'
_chemical_formula_weight         689.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-05-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                86.331(3)
_cell_angle_beta                 82.998(3)
_cell_angle_gamma                86.923(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2887(3)
_cell_length_b                   12.5359(4)
_cell_length_c                   16.8607(5)
_cell_measurement_reflns_used    9162
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.4520
_cell_measurement_theta_min      3.4680
_cell_volume                     1733.44(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -82.00  14.00   1.00    1.00    --  -43.01 104.00 -99.00   96
  2  \w     37.00  64.00   1.00    1.00    --   43.01-104.00 159.00   27
  3  \w     44.00 107.00   1.00    4.00    --  103.80-104.00 159.00   63
  4  \w    111.00 146.00   1.00    4.00    --  103.80 104.00 -99.00   35
  5  \w    -61.00 -25.00   1.00    1.00    --  -43.01 -37.00-180.00   36
  6  \w   -116.00 -73.00   1.00    1.00    --  -43.01 -37.00-180.00   43
  7  \w    -66.00  31.00   1.00    1.00    --  -43.01  37.00-180.00   97
  8  \w     33.00 115.00   1.00    1.00    --   43.01  57.00  30.00   82
  9  \w     29.00  56.00   1.00    1.00    --   43.01 -99.00 -30.00   27
 10  \w     27.00 104.00   1.00    4.00    --  103.80-111.00  90.00   77
 11  \w     24.00 104.00   1.00    4.00    --  103.80 -94.00 -60.00   80
 12  \w     32.00  94.00   1.00    4.00    --  103.80 -61.00 -30.00   62
 13  \w    128.00 172.00   1.00    4.00    --  103.80  45.00 -30.00   44
 14  \w     21.00  64.00   1.00    4.00    --  103.80 -94.00-180.00   43
 15  \w     82.00 107.00   1.00    4.00    --  103.80 -94.00-180.00   25
 16  \w     98.00 177.00   1.00    4.00    --  103.80  45.00 120.00   79
 17  \w     31.00  58.00   1.00    4.00    --  103.80-111.00 -60.00   27
 18  \w     81.00 108.00   1.00    4.00    --  103.80-111.00  60.00   27
 19  \w     27.00  53.00   1.00    4.00    --  103.80-111.00  60.00   26
 20  \w     57.00 129.00   1.00    4.00    --  103.80 -61.00 150.00   72
 21  \w     84.00 111.00   1.00    4.00    --  103.80  45.00 -30.00   27
 22  \w     83.00 108.00   1.00    4.00    --  103.80-111.00 -60.00   25
 23  \w    137.00 170.00   1.00    4.00    --  103.80 111.00-150.00   33
 24  \w     77.00 177.00   1.00    4.00    --  103.80  30.00-120.00  100
 25  \w    132.00 159.00   1.00    4.00    --  103.80  77.00 150.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0822906000
_diffrn_orient_matrix_UB_12      0.0028729000
_diffrn_orient_matrix_UB_13      -0.0773001000
_diffrn_orient_matrix_UB_21      0.1371271000
_diffrn_orient_matrix_UB_22      0.0674751000
_diffrn_orient_matrix_UB_23      -0.0439075000
_diffrn_orient_matrix_UB_31      0.0978040000
_diffrn_orient_matrix_UB_32      -0.1031310000
_diffrn_orient_matrix_UB_33      -0.0244906000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14148
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.576
_diffrn_reflns_theta_min         3.537
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.254
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6693
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0130P)^2^+0.3649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6159
_reflns_number_total             6693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05161j2.cif
_cod_data_source_block           wf446pd
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7129122--7129133.cif.
;
_cod_original_cell_volume        1733.45(9)
_cod_database_code               7129125
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C38 H47 Cl N2 O Pd'
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.331
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9A-C10 \\sim C9B-C10
 with sigma of 0.02
 C9A-C8 \\sim C9B-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C8 \\sim C9A \\sim C9B \\sim C10: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C35A \\sim C35B \\sim C36A \\sim C36B \\sim C37A \\sim C37B \\sim C38A \\sim
C38B \\sim C39A \\sim C39B \\sim C40A \\sim C40B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(H8BC)=Sof(H8BD)=Sof(C9B)=Sof(H9B)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9A)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(C37B)=Sof(H37B)=Sof(C36B)=Sof(H36B)=Sof(C35B)=Sof(H35B)=Sof(C40B)=
 Sof(H40B)=Sof(C39B)=Sof(H39B)=Sof(C38B)=Sof(H38B)=1-FVAR(2)
 Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=
 Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C9A(H9A), C9B(H9B), C17(H17), C20(H20), C29(H29), C32(H32)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8BC,H8BD), C8(H8AA,H8AB), C10(H10C,H10D), C10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C13(H13), C14(H14), C15(H15), C25(H25), C26(H26), C27(H27),
 C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A), C39A(H39A), C40A(H40A),
 C37B(H37B), C36B(H36B), C35B(H35B), C40B(H40B), C39B(H39B), C38B(H38B)
5.d Fitted hexagon refined as free rotating group:
 C37B(C36B,C35B,C40B,C39B,C38B)
5.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C)
;
_shelx_res_checksum              79472
_shelx_hkl_checksum              31965
_olex2_date_sample_data_collection 2021-05-12
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.796