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_7709539
_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_absolute_configuration unk
_chemical_formula_moiety         '2(C32 H28 N16 O8 Sn2)'
_chemical_formula_sum            'C64 H56 N32 O16 Sn4'
_chemical_formula_weight         2004.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
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2021-11-26 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.993(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0397(3)
_cell_length_b                   14.1993(5)
_cell_length_c                   24.7702(8)
_cell_measurement_reflns_used    14840
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.3840
_cell_measurement_theta_min      2.8240
_cell_volume                     3882.3(2)
_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 (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, 2018)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.884
_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    -86.00  13.00   1.00   15.00    --  -11.70 -38.00-150.00   99
  2  \w    -53.00  68.00   1.00   15.00    --  -11.70  19.00  30.00  121
  3  \w    -20.00   5.00   1.00   15.00    --  -11.70 -99.00  60.00   25
  4  \w    -53.00  68.00   1.00   15.00    --  -11.70  19.00-120.00  121
;
_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      -0.0365370000
_diffrn_orient_matrix_UB_12      0.0083659000
_diffrn_orient_matrix_UB_13      -0.0233400000
_diffrn_orient_matrix_UB_21      0.0100129000
_diffrn_orient_matrix_UB_22      -0.0469136000
_diffrn_orient_matrix_UB_23      -0.0086933000
_diffrn_orient_matrix_UB_31      -0.0519140000
_diffrn_orient_matrix_UB_32      -0.0149572000
_diffrn_orient_matrix_UB_33      0.0141397000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            38593
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.831
_diffrn_reflns_theta_min         2.182
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.544
_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    1.714
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.036
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.43(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         18098
_refine_ls_number_restraints     412
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0428
_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^)+(0.0274P)^2^+0.8504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.735
_reflns_number_gt                15800
_reflns_number_total             18098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04040e2.cif
_cod_data_source_block           buni160912
_cod_database_code               7709539
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C72H56N32O16Sn4
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.57(2)
 0.43(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Rigid bond restraints
 N32B, N31B, C32B, C33B, C31B, N32A, N31A, C33A, C31A, C32A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N61, C61, C62, C63, N62
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C51, C52, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N32B \\sim N31B \\sim C32B \\sim C33B \\sim C31B \\sim N32A \\sim N31A \\sim
C33A \\sim H33A \\sim C31A \\sim C32A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C61 \\sim C62 \\sim C63 \\sim N62 \\sim N61: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C52 \\sim C51 \\sim C53: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C61) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(N32B) \\sim Ueq, Uanis(N31B) \\sim Ueq, Uanis(C32B) \\sim Ueq,
Uanis(C33B) \\sim Ueq, Uanis(C31B) \\sim Ueq, Uanis(N32A) \\sim Ueq,
Uanis(N31A) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C31A) \\sim Ueq,
Uanis(C32A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N31B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C63) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C161) \\sim Ueq, Uanis(N161) \\sim Ueq, Uanis(C162) \\sim Ueq,
Uanis(C163) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
5. Rigid body (RIGU) restrains
 N62, N61, C61, C63, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H3B)=Sof(N32A)=Sof(N31A)=Sof(C33A)=Sof(H33A)=Sof(C31A)=Sof(H31A)=
 Sof(C32A)=Sof(H32A)=1-FVAR(1)
 Sof(N32B)=Sof(H3A)=Sof(N31B)=Sof(C32B)=Sof(H32B)=Sof(C33B)=Sof(H33B)=
 Sof(C31B)=Sof(H31B)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C101(H101), C5(H5), C105(H105), C103(H103), C3(H3B), C3(H3A), C7(H7),
 C107(H107)
7.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C51(H51), C42(H42), C13(H13), C111(H111), C43(H43), C143(H143),
 C172(H172), C171(H171), C142(H142), C71(H71), C12(H12), C113(H113), C173(H173),
  C151(H151), C72(H72), C82(H82), C182(H182), C112(H112), C23(H23), C61(H61),
 C73(H73), C83(H83), C183(H183), C123(H123), C161(H161), C133(H133), C21(H21),
 C63(H63), C121(H121), C162(H162), C122(H122), C163(H163), C132(H132), C53(H53),
  C62(H62), C52(H52), C81(H81), C41(H41), C22(H22), C32B(H32B), C152(H152),
 C181(H181), C153(H153), C141(H141), C131(H131), C33B(H33B), C31B(H31B),
 C33A(H33A), C31A(H31A), C32A(H32A)
;
_shelx_res_checksum              91485
_shelx_hkl_checksum              34635
_olex2_date_sample_data_collection 2016-09-12
_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 1.607
_oxdiff_exptl_absorpt_empirical_full_min 0.737