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_7129132
_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         'C29 H36 Cl3 Ga N2 O, 0.5 (C7 H7)'
_chemical_formula_sum            'C32.5 H39.5 Cl3 Ga N2 O'
_chemical_formula_weight         650.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-05-12
_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                90
_cell_angle_beta                 100.7901(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.39335(14)
_cell_length_b                   19.4815(2)
_cell_length_c                   16.5164(2)
_cell_measurement_reflns_used    14839
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.4990
_cell_measurement_theta_min      3.4920
_cell_volume                     3285.08(7)
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_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   -120.00  -9.00   1.00    6.00    --  -43.13 -24.00 -86.00  111
  2  \w    -25.00  35.00   1.00    6.00    --  -43.13  24.00  77.00   60
  3  \w     70.00 121.00   1.00    6.00    --   43.13  24.00  77.00   51
  4  \w     27.00  64.00   1.00    6.00    --   43.13 -24.00 -86.00   37
  5  \w     60.00  86.00   1.00   24.00    --  103.80 -24.00 -86.00   26
  6  \w     70.00 164.00   1.00   24.00    --  103.80  24.00  77.00   94
  7  \w    -61.00 -18.00   1.00    6.00    --  -43.13 125.00 150.00   43
  8  \w     74.00  99.00   1.00    6.00    --   43.13-125.00   0.00   25
  9  \w     28.00  82.00   1.00    6.00    --   43.13 -99.00 -30.00   54
 10  \w     30.00  98.00   1.00    6.00    --   43.13-125.00-150.00   68
 11  \w     76.00 108.00   1.00   24.00    --  103.80-111.00 120.00   32
 12  \w    132.00 163.00   1.00   24.00    --  103.80  77.00 -90.00   31
 13  \w    103.00 177.00   1.00   24.00    --  103.80  77.00 -30.00   74
 14  \w    103.00 176.00   1.00   24.00    --  103.80  77.00 120.00   73
 15  \w    111.00 177.00   1.00   24.00    --  103.80 111.00   0.00   66
 16  \w     36.00  62.00   1.00   24.00    --  103.80-111.00 120.00   26
 17  \w     52.00  78.00   1.00   24.00    --  103.80-111.00-150.00   26
 18  \w    103.00 177.00   1.00   24.00    --  103.80  77.00  90.00   74
 19  \w     31.00  58.00   1.00   24.00    --  103.80-111.00 -60.00   27
 20  \w     74.00 100.00   1.00   24.00    --  103.80-111.00 -60.00   26
 21  \w     53.00 106.00   1.00   24.00    --  103.80 -94.00   0.00   53
 22  \w     44.00 133.00   1.00   24.00    --  103.80 -61.00   0.00   89
 23  \w     37.00 107.00   1.00   24.00    --  103.80 -94.00 -60.00   70
 24  \w     26.00 108.00   1.00   24.00    --  103.80-103.00-167.26   82
 25  \w     44.00  69.00   1.00   24.00    --  103.80 -94.00 150.00   25
;
_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      0.1172488000
_diffrn_orient_matrix_UB_12      0.0247032000
_diffrn_orient_matrix_UB_13      0.0648253000
_diffrn_orient_matrix_UB_21      -0.0856212000
_diffrn_orient_matrix_UB_22      -0.0022340000
_diffrn_orient_matrix_UB_23      0.0666966000
_diffrn_orient_matrix_UB_31      0.0411694000
_diffrn_orient_matrix_UB_32      -0.0750399000
_diffrn_orient_matrix_UB_33      0.0193594000
_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  0.0304
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28001
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.609
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.593
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.654
_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 pale yellow'
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       plate
_exptl_crystal_F_000             1354
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6441
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0474P)^2^+1.3924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5515
_reflns_number_total             6441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05161j2.cif
_cod_data_source_block           wf446gacl3
_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_formula_sum        'C32.50 H39.50 Cl3 Ga N2 O'
_cod_database_code               7129132
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C32.50 H39.50 Cl3 Ga N2 O'
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.580
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Ga1-Cl1A \\sim Ga1-Cl1B \\sim Ga1-Cl3A \\sim Ga1-Cl3B \\sim Ga1-Cl2B \\sim
Ga1-Cl2A
 with sigma of 0.02
 Cl1A-Cl2A \\sim Cl2A-Cl3A \\sim Cl3A-Cl1A
 with sigma of 0.02
 Cl2B-Cl1B \\sim Cl1B-Cl3B \\sim Cl3B-Cl2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C32 \\sim C33 \\sim C34 \\sim C35: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(Cl1A) = Uanis(Cl1B)
Uanis(Cl3A) = Uanis(Cl3B)
4. Others
 Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=FVAR(1)
 Fixed Sof: C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C26(H26), C29(H29)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C22(H22), C23(H23), C24(H24),
 C33(H33), C34(H34)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              42473
_shelx_hkl_checksum              49929
_olex2_date_sample_data_collection 2021-05-10
_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 1.184
_oxdiff_exptl_absorpt_empirical_full_min 0.834