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_7709538
_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         'C24 H30 Ga N8 O4, Cl O4, C H2 Cl2'
_chemical_formula_sum            'C25 H32 Cl3 Ga N8 O8'
_chemical_formula_weight         748.65
_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
_audit_creation_date             2017-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2021-10-21 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
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_cell_angle_alpha                101.090(4)
_cell_angle_beta                 103.231(4)
_cell_angle_gamma                106.077(4)
_cell_formula_units_Z            2
_cell_length_a                   9.7565(5)
_cell_length_b                   12.3535(6)
_cell_length_c                   14.4351(7)
_cell_measurement_reflns_used    7904
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.3260
_cell_measurement_theta_min      3.8860
_cell_volume                     1565.39(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_details
;
  1 omega  -85.00   17.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.3916  -57.0000   30.0000 102

  2 omega  -40.00   62.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.3916   57.0000 -180.0000 102

  3 omega  -16.00   85.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0166   57.0000  -30.0000 101

  4 omega  -62.00   37.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0166  -38.0000  -30.0000 99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0228118000
_diffrn_orient_matrix_UB_12      -0.0400362000
_diffrn_orient_matrix_UB_13      0.0272676000
_diffrn_orient_matrix_UB_21      0.0529374000
_diffrn_orient_matrix_UB_22      -0.0265199000
_diffrn_orient_matrix_UB_23      -0.0097434000
_diffrn_orient_matrix_UB_31      0.0544474000
_diffrn_orient_matrix_UB_32      0.0394057000
_diffrn_orient_matrix_UB_33      0.0437645000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17048
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.608
_diffrn_reflns_theta_min         3.014
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.4462
_exptl_crystal_size_mid          0.1945
_exptl_crystal_size_min          0.0672
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0276P)^2^+1.0502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6546
_reflns_number_total             7502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04040e2.cif
_cod_data_source_block           buni160913a
_cod_original_cell_volume        1565.38(14)
_cod_database_code               7709538
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Cl Ga'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Others
 Sof(H91C)=Sof(H91D)=Sof(Cl3B)=1-FVAR(1)
 Sof(Cl3A)=Sof(H91A)=Sof(H91B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C3(H3), C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C91(H91A,H91B), C91(H91C,H91D)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C42(H42), C22(H22), C32(H32)
3.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C81(H81A,H81B,H81C), C61(H61A,H61B,H61C), C62(H62A,H62B,
 H62C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C52(H52A,H52B,H52C), C82(H82A,
 H82B,H82C)
;
_olex2_date_sample_data_collection 2016-09-13
_olex2_submission_special_instructions 'No special instructions were received'