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_7704905
_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         'C58 H78 Ca N4 O Sn'
_chemical_formula_sum            'C58 H78 Ca N4 O Sn'
_chemical_formula_weight         1006.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-12 deposited with the CCDC.	2020-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.881(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.2727(4)
_cell_length_b                   29.2030(4)
_cell_length_c                   29.1410(5)
_cell_measurement_reflns_used    17642
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.8920
_cell_measurement_theta_min      3.4020
_cell_volume                     21956.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            58687
_diffrn_reflns_point_group_measured_fraction_full 0.718
_diffrn_reflns_point_group_measured_fraction_max 0.717
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         2.934
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.821
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.217
_exptl_crystal_description       plate
_exptl_crystal_F_000             8512
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.929
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 5802 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.044(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2413
_refine_ls_number_reflns         28831
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0808P)^2^+11.5460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1730
_reflns_Friedel_coverage         0.442
_reflns_Friedel_fraction_full    0.442
_reflns_Friedel_fraction_max     0.440
_reflns_number_gt                23442
_reflns_number_total             28831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02406f2.cif
_cod_data_source_block           s20msh17-Cpd-13THF
_cod_depositor_comments
;Adding full bibliography for 7704902--7704908.cif.

 Adding full bibliography for 7704902--7704908.cif.
;
_cod_database_code               7704905
_shelxl_version_number           2014-3
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28), C32(H32), C35(H35), C129(H129),
 C132(H132), C141(H141), C144(H144), C148(H148), C151(H151), C71(H71), C74(H74),
  C83(H83), C86(H86), C90(H90), C93(H93), C187(H187), C190(H190), C199(H199),
 C202(H202), C206(H206), C209(H209)
2.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C171(H17D,
 H17E), C172(H17F,H17G), C173(H17H,H17I), C174(H17J,H17K), C113(H11A,H11B),
 C114(H11C,H11D), C115(H11E,H11F), C116(H11G,H11H), C03J(H03A,H03B), C05A(H05A,
 H05B), C06A(H06A,H06B), C020(H02A,H02B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
  C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C124(H124), C125(H125),
 C126(H126), C136(H136), C137(H137), C138(H138), C154(H154), C155(H155),
 C156(H156), C157(H157), C158(H158), C160(H160), C161(H161), C162(H162),
 C163(H163), C164(H164), C166(H166), C167(H167), C168(H168), C169(H169),
 C170(H170), C66(H66), C67(H67), C68(H68), C78(H78), C79(H79), C80(H80),
 C96(H96), C97(H97), C98(H98), C99(H99), C100(H100), C102(H102), C103(H103),
 C104(H104), C105(H105), C106(H106), C108(H108), C109(H109), C110(H110),
 C111(H111), C112(H112), C182(H182), C183(H183), C184(H184), C194(H194),
 C195(H195), C196(H196), C212(H212), C213(H213), C214(H214), C215(H215),
 C216(H216), C218(H218), C219(H219), C220(H220), C221(H221), C222(H222),
 C224(H224), C225(H225), C226(H226), C227(H227), C228(H228)
2.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), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C117(H11I,H11J,H11K),
 C121(H12D,H12E,H12F), C128(H12G,H12H,H12I), C130(H13A,H13B,H13C), C131(H13D,
 H13E,H13F), C133(H13G,H13H,H13I), C140(H14D,H14E,H14F), C142(H14G,H14H,H14I),
 C143(H14J,H14K,H14L), C145(H14M,H14N,H14O), C147(H14P,H14Q,H14R), C149(H14S,
 H14T,H14U), C150(H15D,H15E,H15F), C152(H15G,H15H,H15I), C59(H59A,H59B,H59C),
 C63(H63A,H63B,H63C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,
 H73C), C75(H75A,H75B,H75C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C85(H85A,
 H85B,H85C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C), C91(H91A,H91B,H91C),
 C92(H92A,H92B,H92C), C94(H94A,H94B,H94C), C175(H17L,H17M,H17N), C179(H17O,H17P,
 H17Q), C186(H18A,H18B,H18C), C188(H18D,H18E,H18F), C189(H18G,H18H,H18I),
 C191(H19A,H19B,H19C), C198(H19D,H19E,H19F), C200(H20A,H20B,H20C), C201(H20D,
 H20E,H20F), C203(H20G,H20H,H20I), C205(H20J,H20K,H20L), C207(H20M,H20N,H20O),
 C208(H20P,H20Q,H20R), C210(H21A,H21B,H21C)
;