p-Block metal complexes with bis(pyrazol-1-yl)acetato ligands
Pflock, Stephan; Langer, Frauke; Reil, Michaela; Strinitz, Lisa; Lorenz, Rebecca; Hübner, Eike G.; Burzlaff, Nicolai; Dalton Transactions  (2022) –; doi:10.1039/D1DT04040E

data_7709537
_publ_section_title
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 &#x000D; p-Block metal complexes with bis(pyrazol-1-yl)acetato ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04040E
_journal_year                    2022
_chemical_formula_moiety         'Cl4 Ga, C16 H14 Ga N8 O4'
_chemical_formula_sum            'C16 H14 Cl4 Ga2 N8 O4'
_chemical_formula_weight         663.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-30
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-21 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.304(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0141(5)
_cell_length_b                   8.3409(3)
_cell_length_c                   16.4275(6)
_cell_measurement_reflns_used    3547
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      72.5030
_cell_measurement_theta_min      5.1940
_cell_volume                     2330.67(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_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   -114.00 -13.00   1.00    3.00    --  -41.48 -57.00  30.00  101
  2  \w    -21.00  74.00   1.00    3.00    --   41.48 -77.00-120.00   95
  3  \w     29.00  99.00   1.00    3.00    --   41.48-127.00 155.00   70
  4  \w     31.00 112.00   1.00   12.00    --  104.33-125.00  30.00   81
  5  \w     28.00 133.00   1.00   12.00    --  104.33 -30.00 150.00  105
  6  \w     22.00 106.00   1.00   12.00    --  104.33 -94.00-150.00   84
  7  \w    103.00 178.00   1.00   12.00    --  104.33  77.00 150.00   75
  8  \w     22.00 106.00   1.00   12.00    --  104.33 -94.00 -60.00   84
  9  \w     75.00 177.00   1.00   12.00    --  104.33  61.00 -60.00  102
 10  \w   -116.00 -17.00   1.00    3.00    --  -41.48 -38.00 120.00   99
 11  \w     13.00 114.00   1.00    3.00    --   41.48  57.00-120.00  101
 12  \w    103.00 128.00   1.00   12.00    --  104.33  77.00-150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0882489000
_diffrn_orient_matrix_UB_12      -0.0413830000
_diffrn_orient_matrix_UB_13      -0.0023436000
_diffrn_orient_matrix_UB_21      0.0199363000
_diffrn_orient_matrix_UB_22      0.1796549000
_diffrn_orient_matrix_UB_23      -0.0055563000
_diffrn_orient_matrix_UB_31      0.0054328000
_diffrn_orient_matrix_UB_32      0.0098211000
_diffrn_orient_matrix_UB_33      0.0935833000
_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  0.0296
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6667
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.804
_diffrn_reflns_theta_min         5.201
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.446
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0377P)^2^+4.4192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2075
_reflns_number_total             2241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04040e2.cif
_cod_data_source_block           buni210309a
_cod_original_cell_volume        2330.68(14)
_cod_database_code               7709537
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Ga Cl'
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.184
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C22(H22), C24(H24), C12(H12), C13(H13), C23(H23)
;
_shelx_res_checksum              17277
_shelx_hkl_checksum              86088
_olex2_date_sample_data_collection 2021-03-09
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.091
_oxdiff_exptl_absorpt_empirical_full_min 0.664