Synthesis and reactivity of alkaline-earth stannanide complexes by hydride-mediated distannane metathesis and organostannane dehydrogenation.
Morris, Louis J.; Rajabi, Nasir A.; Mahon, Mary F.; Manners, Ian; McMullin, Claire L.; Hill, Michael S.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10523–10534; doi:10.1039/d0dt02406f

data_7704908
_publ_section_title
;
 Synthesis and reactivity of alkaline-earth stannanide complexes by
 hydride-mediated distannane metathesis and organostannane
 dehydrogenation.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10523
_journal_page_last               10534
_journal_paper_doi               10.1039/d0dt02406f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '4(C44 H48 Sn3)'
_chemical_formula_sum            'C176 H192 Sn12'
_chemical_formula_weight         3731.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-09
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-05-12 deposited with the CCDC.	2020-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.4180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   20.3538(2)
_cell_length_b                   10.40690(10)
_cell_length_c                   20.6522(2)
_cell_measurement_reflns_used    26478
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.9370
_cell_measurement_theta_min      4.3240
_cell_volume                     4014.22(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54559
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.134
_diffrn_reflns_theta_min         4.312
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.926
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8008
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0562P)^2^+2.9489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7434
_reflns_number_total             8008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02406f2.cif
_cod_data_source_block           s20msh7-Cpd-11
_cod_depositor_comments
;Adding full bibliography for 7704902--7704908.cif.

 Adding full bibliography for 7704902--7704908.cif.
;
_cod_original_cell_volume        4014.21(7)
_cod_database_code               7704908
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C20A-C19 \\sim C20B-C19 \\sim C21A-C19 \\sim C21B-C19 \\sim C22A-C19 \\sim
C22B-C19
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C20B \\sim C21B \\sim C22B \\sim C20A \\sim C21A \\sim C22A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: C20B(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C21B(0.5) H21A(0.5)
 H21B(0.5) H21C(0.5) C22B(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C20A(0.5)
 H20D(0.5) H20E(0.5) H20F(0.5) C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5)
 C22A(0.5) H22D(0.5) H22E(0.5) H22F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C28(H28), C29(H29),
  C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
5.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C20B(H20A,H20B,
 H20C), C21B(H21A,H21B,H21C), C22B(H22A,H22B,H22C), C20A(H20D,H20E,H20F),
 C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              12693