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_7704902
_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         'C65 H71 Ca N2 O P Sn'
_chemical_formula_sum            'C65 H71 Ca N2 O P Sn'
_chemical_formula_weight         1085.97
_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             2019-03-05
_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                 103.5090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.80860(10)
_cell_length_b                   16.66720(10)
_cell_length_c                   25.6761(2)
_cell_measurement_reflns_used    30505
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3370
_cell_measurement_theta_min      4.2730
_cell_volume                     5745.88(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'olex2.solve (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 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, 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  0.0532
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            76338
_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         73.435
_diffrn_reflns_theta_min         3.188
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.895
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         11514
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0337P)^2^+1.8644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9840
_reflns_number_total             11514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02406f2.cif
_cod_data_source_block           s19msh34-Cpd-8OPPh3
_cod_depositor_comments
;Adding full bibliography for 7704902--7704908.cif.

 Adding full bibliography for 7704902--7704908.cif.
;
_cod_database_code               7704902
_shelxl_version_number           2014-3
_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
 C27-H27A = C27-H27B = C27-H27C
 0.98 with sigma of 0.005
 C28-H28
 0.98 with sigma of 0.005
 C19-C24 \\sim C19-C24A
 with sigma of 0.02
 C26-C24 \\sim C26A-C24A
 with sigma of 0.02
 C24-C25 \\sim C24A-C25A
 with sigma of 0.02
 C19-C26 \\sim C19-C26A
 with sigma of 0.04
 C19-C25 \\sim C19-C25A
 with sigma of 0.04
 C26-C25 \\sim C26A-C25A
 with sigma of 0.04
 C24-C19 \\sim C24A-C19
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C24A) = Uanis(C24)
4. Others
 Fixed Sof: C24(0.7) H24(0.7) C25(0.7) H25A(0.7) H25B(0.7) H25C(0.7) C26(0.7)
 H26A(0.7) H26B(0.7) H26C(0.7) C24A(0.3) H24A(0.3) C25A(0.3) H25D(0.3)
 H25F(0.3) H25E(0.3) C26A(0.3) H26E(0.3) H26D(0.3) H26F(0.3)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C24(H24), C24A(H24A)
5.b 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), C49(H49), C50(H50),
 C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
  C61(H61), C62(H62), C63(H63), C64(H64), C65(H65)
5.c 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), C29(H29A,H29B,H29C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C25A(H25D,H25F,H25E), C26A(H26E,H26D,H26F)
;