Calcium Stannyl Formation by Organostannane Dehydrogenation
Hill, Michael; Morris, Louis; McMullin, Claire L.; Mahon, Mary F.; Rajabi, Nasir A.; Manners, Ian; Chemical Communications  (2019) –; doi:10.1039/C9CC07289F

data_7124269
_publ_section_title
;
 Calcium Stannyl Formation by Organostannane Dehydrogenation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07289F
_journal_year                    2019
_chemical_formula_moiety         'C76 H98 Ca2 N4 Sn, 0.5(C6 H14), C7 H8'
_chemical_formula_sum            'C86 H113 Ca2 N4 Sn'
_chemical_formula_weight         1401.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-03 deposited with the CCDC.    2019-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.5230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4972(2)
_cell_length_b                   15.15460(10)
_cell_length_c                   24.4653(2)
_cell_measurement_reflns_used    47882
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.0220
_cell_measurement_theta_min      3.4220
_cell_volume                     7926.01(12)
_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 0.996
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            110586
_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         73.086
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.022
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.872
_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    1.175
_exptl_crystal_description       block
_exptl_crystal_F_000             2988
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.049
_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     892
_refine_ls_number_reflns         15819
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0440P)^2^+4.2518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14145
_reflns_number_total             15819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07289f2.cif
_cod_data_source_block           s18msh155-cpd-3
_cod_original_cell_volume        7926.00(12)
_cod_database_code               7124269
_shelxl_version_number           2014-3
_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. Restrained distances
 C84-C83 = C85-C84 = C87-C86 = C86-C85 = C88-C87
 1.54 with sigma of 0.01
 C83-C84 \\sim C84-C85 \\sim C85-C86 \\sim C86-C87 \\sim C87-C88
 with sigma of 0.02
 C83-C85 \\sim C85-C87 \\sim C84-C86 \\sim C86-C88
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01
C83 \\sim C88: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C83, C84, C85, C86, C87, C88
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5) C84(0.5) H84A(0.5)
 H84B(0.5) C85(0.5) H85A(0.5) H85B(0.5) C86(0.5) H86A(0.5) H86B(0.5) C87(0.5)
 H87A(0.5) H87B(0.5) C88(0.5) H88A(0.5) H88B(0.5) H88C(0.5)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28), C41(H41), C44(H44), C53(H53), C56(H56)
6.b Secondary CH2 refined with riding coordinates:
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C012(H012), C20(H20), C21(H21), C22(H22),
 C36(H36), C37(H37), C38(H38), C48(H48), C49(H49), C50(H50), C59(H59), C60(H60),
  C61(H61), C62(H62), C63(H63), C65(H65), C66(H66), C67(H67), C68(H68),
 C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C77(H77), C78(H78),
  C79(H79), C80(H80), C81(H81)
6.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), C30(H30A,H30B,H30C), C33(H33A,
 H33B,H33C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C45(H45A,H45B,H45C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C57(H57A,H57B,H57C), C83(H83A,H83B,H83C), C88(H88A,H88B,H88C), C82(H82A,
 H82B,H82C)
;