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_7704904
_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         'C55 H72 Ca N2 O2 Sn'
_chemical_formula_sum            'C55 H72 Ca N2 O2 Sn'
_chemical_formula_weight         951.91
_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             2019-12-13
_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                 109.1430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.28860(10)
_cell_length_b                   39.8390(3)
_cell_length_c                   10.83750(10)
_cell_measurement_reflns_used    31847
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.8020
_cell_measurement_theta_min      3.8060
_cell_volume                     5012.28(8)
_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      150.00(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 0.998
_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  0.0521
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            64874
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.875
_diffrn_reflns_theta_min         3.808
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.255
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72704
_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    1.261
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         9977
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0639P)^2^+4.2639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9253
_reflns_number_total             9977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02406f2.cif
_cod_data_source_block           s19msh185-Cpd-8(THF)2
_cod_depositor_comments
;Adding full bibliography for 7704902--7704908.cif.

 Adding full bibliography for 7704902--7704908.cif.
;
_cod_database_code               7704904
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     'colourless plate'
_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. Restrained distances
 O2-C52 \\sim O2-C52A \\sim O2-C55 \\sim O1-C51 \\sim O1-C48
 with sigma of 0.005
 C54A-C53A \\sim C54-C53 \\sim C50-C49 \\sim C50A-C49A
 with sigma of 0.005
 C53-C52 \\sim C53A-C52A \\sim C55-C54A \\sim C55-C54 \\sim C51-C50 \\sim
C51-C50A \\sim C49A-C48 
 C49-C48
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C50A) = Uanis(C50)
Uanis(C52) = Uanis(C52A)
Uanis(C54) = Uanis(C54A)
Uanis(C53A) = Uanis(C53)
4. Others
 Fixed Sof: H48A(0.75) H48B(0.75) H48C(0.25) H48D(0.25) H51A(0.75) H51B(0.75)
 H51C(0.25) H51D(0.25) H55A(0.65) H55B(0.65) H55C(0.35) H55D(0.35) C49(0.75)
 H49A(0.75) H49B(0.75) C50(0.75) H50A(0.75) H50B(0.75) C52(0.65) H52A(0.65)
 H52B(0.65) C53(0.65) H53A(0.65) H53B(0.65) C54(0.65) H54A(0.65) H54B(0.65)
 C49A(0.25) H49C(0.25) H49D(0.25) C50A(0.25) H50C(0.25) H50D(0.25) C52A(0.35)
 H52C(0.35) H52D(0.35) C53A(0.35) H53C(0.35) H53D(0.35) C54A(0.35) H54C(0.35)
 H54D(0.35)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C48(H48C,H48D), C51(H51A,H51B), C51(H51C,H51D), C55(H55A,
 H55B), C55(H55C,H55D), C49(H49A,H49B), C50(H50A,H50B), C52(H52A,H52B),
 C53(H53A,H53B), C54(H54A,H54B), C49A(H49C,H49D), C50A(H50C,H50D), C52A(H52C,
 H52D), C53A(H53C,H53D), C54A(H54C,H54D)
5.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)
5.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              75278