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_7709535
_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 N8 O4 Sn'
_chemical_formula_sum            'C24 H30 N8 O4 Sn'
_chemical_formula_weight         613.25
_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     direct
_audit_creation_date             2017-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2021-10-21 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.184(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2234(3)
_cell_length_b                   22.7396(7)
_cell_length_c                   14.1698(5)
_cell_measurement_reflns_used    5796
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      29.3280
_cell_measurement_theta_min      3.6350
_cell_volume                     2615.74(16)
_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      100.0(2)
_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 0.998
_diffrn_measurement_details
;
  1 omega  -12.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2510   38.0000   90.0000 99

  2 omega  -62.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2510  -38.0000  -90.0000 99

  3 omega   34.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2510 -178.0000  150.0000 58
;
_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      -0.0501443000
_diffrn_orient_matrix_UB_12      0.0191888000
_diffrn_orient_matrix_UB_13      0.0224237000
_diffrn_orient_matrix_UB_21      -0.0616377000
_diffrn_orient_matrix_UB_22      -0.0220208000
_diffrn_orient_matrix_UB_23      -0.0030438000
_diffrn_orient_matrix_UB_31      0.0363450000
_diffrn_orient_matrix_UB_32      -0.0109854000
_diffrn_orient_matrix_UB_33      0.0453623000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7893
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.040
_diffrn_reflns_theta_min         2.912
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.953
_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    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.2565
_exptl_crystal_size_mid          0.1645
_exptl_crystal_size_min          0.1024
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+3.1448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2466
_reflns_number_total             2586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04040e2.cif
_cod_data_source_block           buni160224a
_cod_original_cell_volume        2615.73(15)
_cod_database_code               7709535
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Sn'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.00
_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), C42(H42A,H42B,H42C), C32(H32A,H32B,H32C), C31(H31A,H31B,
 H31C)
;
_olex2_date_sample_data_collection 2016-02-24
_olex2_submission_special_instructions 'No special instructions were received'