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_7709536
_publ_section_title
;
 &#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         'C12 H15 F3 N4 O2 Sn'
_chemical_formula_sum            'C12 H15 F3 N4 O2 Sn'
_chemical_formula_weight         422.97
_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
_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.
;
_cell_angle_alpha                110.060(5)
_cell_angle_beta                 98.633(4)
_cell_angle_gamma                106.314(5)
_cell_formula_units_Z            2
_cell_length_a                   8.1077(4)
_cell_length_b                   8.4826(5)
_cell_length_c                   11.9826(6)
_cell_measurement_reflns_used    5556
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.3310
_cell_measurement_theta_min      3.4240
_cell_volume                     714.63(8)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(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 0.859
_diffrn_measurement_details
;
  1 omega  -40.00   61.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7041   57.0000  120.0000 101

  2 omega  -85.00   16.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7041  -57.0000  -30.0000 101

  3 omega  -20.00   88.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1728   77.0000 -120.0000 108

  4 omega  -86.00  -31.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7041  -38.0000   60.0000 55

  5 omega  -20.00   53.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1728  -99.0000  -90.0000 73

  6 omega   34.00   99.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1728 -178.0000   90.0000 65
;
_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      0.0211499000
_diffrn_orient_matrix_UB_12      -0.0722882000
_diffrn_orient_matrix_UB_13      0.0070958000
_diffrn_orient_matrix_UB_21      0.0888774000
_diffrn_orient_matrix_UB_22      0.0590648000
_diffrn_orient_matrix_UB_23      0.0332691000
_diffrn_orient_matrix_UB_31      -0.0251770000
_diffrn_orient_matrix_UB_32      0.0193469000
_diffrn_orient_matrix_UB_33      0.0559893000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9668
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.753
_diffrn_reflns_theta_min         3.093
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.835
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.936
_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    1.966
_exptl_crystal_description       block
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.0874
_exptl_crystal_size_mid          0.0716
_exptl_crystal_size_min          0.0529
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0150P)^2^+0.2722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3226
_reflns_number_total             3505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04040e2.cif
_cod_data_source_block           buni160816a
_cod_original_cell_volume        714.63(7)
_cod_database_code               7709536
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Sn B F Cl'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C12(H12)
2.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C42(H42A,H42B,
 H42C)
;
_olex2_date_sample_data_collection 2016-08-16
_olex2_submission_special_instructions 'No special instructions were received'