Pyridylpyrrolido ligand in Ge(ii) and Sn(ii) chemistry: synthesis, reactivity and catalytic application
Pahar, Sanjukta; Sharma, Vishal; Tothadi, Srinu; Sen, Sakya S.; Dalton Transactions  (2021) –; doi:10.1039/D1DT03136H

data_7708781
_publ_section_title
;
 Pyridylpyrrolido ligand in Ge(ii) and Sn(ii) chemistry: synthesis,
 reactivity and catalytic application
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03136H
_journal_year                    2021
_chemical_formula_moiety         'C22 H22 N4 Sn'
_chemical_formula_sum            'C22 H22 N4 Sn'
_chemical_formula_weight         461.15
_chemical_name_systematic        Homoleptic_Sn
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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     heavy
_audit_block_doi                 10.5517/ccdc.csd.cc28t8r4
_audit_creation_date             2021-09-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-13 deposited with the CCDC.	2021-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                91.477(2)
_cell_angle_beta                 103.126(2)
_cell_angle_gamma                90.790(2)
_cell_formula_units_Z            4
_cell_length_a                   11.9136(7)
_cell_length_b                   12.1859(7)
_cell_length_c                   13.5673(8)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.24
_cell_volume                     1917.18(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41117
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.542
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0758 before and 0.0621 after correction.
The Ratio of minimum to maximum transmission is 0.9276.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       plate
_exptl_crystal_F_000             928.0
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.268
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0491
_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^)+5.9836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7299
_reflns_number_total             8809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03136h2.cif
_cod_data_source_block           sp_a
_cod_database_code               7708781
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Others
 Fixed Sof: Sn(0.75) Sn2(0.25)
2.a Aromatic/amide H refined with riding coordinates:
 C37(H37), C40(H40), C6(H6), C9(H9), C8(H8), C7(H7), C38(H38), C31(H31),
 C2(H2), C30(H30), C11(H11), C39(H39), C33(H33), C28(H28), C24(H24), C29(H29),
 C15(H15), C18(H18), C17(H17), C16(H16)
2.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C19(H19A,H19B,H19C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C41(H41A,
 H41B,H41C)
;
_shelx_res_checksum              68341
_shelx_hkl_checksum              86868
_olex2_submission_original_sample_id 'Homoleptic_sp_a '
_olex2_submission_special_instructions 'No special instructions were received'