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_7704903
_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         'C51 H64 Mg N2 O Sn'
_chemical_formula_sum            'C51 H64 Mg N2 O Sn'
_chemical_formula_weight         864.04
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-17
_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                 91.9625(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.75040(6)
_cell_length_b                   19.53398(9)
_cell_length_c                   20.68576(10)
_cell_measurement_reflns_used    36894
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.9940
_cell_measurement_theta_min      3.7600
_cell_volume                     4745.26(4)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_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 0.997
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67192
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.094
_diffrn_reflns_theta_min         3.112
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.677
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72836
_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            colorless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         9472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+2.2329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8952
_reflns_number_total             9472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02406f2.cif
_cod_data_source_block           s19msh188-Cpd-9THF
_cod_depositor_comments
;Adding full bibliography for 7704902--7704908.cif.

 Adding full bibliography for 7704902--7704908.cif.
;
_cod_database_code               7704903
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H48A(0.66667) H48B(0.66667) H48C(0.33333) H48D(0.33333)
 H51A(0.66667) H51B(0.66667) H51C(0.33333) H51D(0.33333) C49(0.66667)
 H49A(0.66667) H49B(0.66667) C50(0.66667) H50A(0.66667) H50B(0.66667)
 C49A(0.33333) H49C(0.33333) H49D(0.33333) C50A(0.33333) H50C(0.33333)
 H50D(0.33333)
3.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C48(H48C,H48D), C51(H51A,H51B), C51(H51C,H51D), C49(H49A,
 H49B), C50(H50A,H50B), C49A(H49C,H49D), C50A(H50C,H50D)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C43(H43), C44(H44), C45(H45), C46(H46), C47(H47)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              76134