Impact of a rigid backbone on the structure of an agostically-stabilised dialkylstannylene: isolation of an unusual bridged stannyl-stannylene
Keith Izod; Casey M. Dixon; Ross W. Harrington; Michael R. Probert; Chem.Commun. 51 (2015) 679–; doi:10.1039/C4cc08740B

data_7116409
_publ_section_title
;
 Impact of a rigid backbone on the structure of an agostically-stabilised
 dialkylstannylene: isolation of an unusual bridged stannyl-stannylene
;
_journal_name_full               Chem.Commun.
_journal_page_first              679
_journal_paper_doi               10.1039/C4cc08740B
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         '2(C64 H112 B4 P4 Sn2), 3(C7 H8)'
_chemical_formula_sum            'C149 H248 B8 P8 Sn4'
_chemical_formula_weight         2848.46
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Heat-sensitive, Oxygen-sensitive, Light-sensitive, Photo-sensitive'
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.2730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.08850(10)
_cell_length_b                   26.5770(2)
_cell_length_c                   20.0509(2)
_cell_measurement_reflns_used    52081
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.5874
_cell_measurement_theta_min      2.8362
_cell_volume                     7475.89(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0053472000
_diffrn_orient_matrix_UB_12      0.0154522000
_diffrn_orient_matrix_UB_13      0.0282445000
_diffrn_orient_matrix_UB_21      -0.0150412000
_diffrn_orient_matrix_UB_22      -0.0212034000
_diffrn_orient_matrix_UB_23      0.0177799000
_diffrn_orient_matrix_UB_31      0.0479721000
_diffrn_orient_matrix_UB_32      -0.0049013000
_diffrn_orient_matrix_UB_33      0.0121699000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            108054
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.650
_diffrn_reflns_theta_min         2.842
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             3004
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         17595
_refine_ls_number_restraints     782
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+6.3464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14915
_reflns_number_total             17595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08740b2.cif
_cod_data_source_block           compound
_cod_database_code               7116409
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C32 H56 B2 P2 Sn'
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.797
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Others
 Fixed Sof: C1T(0.5) H1TA(0.5) H1TB(0.5) H1TC(0.5) C2T(0.5) C7T(0.5) H7T(0.5)
 C6T(0.5) H6T(0.5) C5T(0.5) H5T(0.5) C4T(0.5) H4T(0.5) C3T(0.5) H3T(0.5)
 C8T(0.622) H8TA(0.622) H8TB(0.622) H8TC(0.622) C9T(0.622) C10T(0.622)
 H10T(0.622) C11T(0.622) H11T(0.622) C12T(0.622) H12T(0.622) C20T(0.622)
 H20T(0.622) C21T(0.622) H21T(0.622) C14T(0.378) H14C(0.378) H14D(0.378)
 H14E(0.378) C15T(0.378) C13T(0.378) H13T(0.378) C19T(0.378) H19T(0.378)
 C18T(0.378) H18T(0.378) C17T(0.378) H17T(0.378) C16T(0.378) H16T(0.378)
 Fixed Uiso: H1(0.018) H3(0.024) H4(0.029) H5(0.028) H6(0.023) H8(0.016)
 H9(0.025) H10A(0.034) H10B(0.034) H11A(0.048) H11B(0.048) H12A(0.06)
 H12B(0.06) H13A(0.05) H13B(0.05) H14A(0.038) H14B(0.038) H15(0.023)
 H16A(0.027) H16B(0.027) H17A(0.033) H17B(0.033) H18A(0.042) H18B(0.042)
 H19A(0.039) H19B(0.039) H20A(0.029) H20B(0.029) H21(0.022) H22A(0.028)
 H22B(0.028) H23A(0.036) H23B(0.036) H24A(0.039) H24B(0.039) H25A(0.037)
 H25B(0.037) H26A(0.029) H26B(0.029) H27(0.022) H28A(0.028) H28B(0.028)
 H29A(0.036) H29B(0.036) H30A(0.038) H30B(0.038) H31A(0.033) H31B(0.033)
 H32A(0.025) H32B(0.025) H33(0.017) H35(0.024) H36(0.03) H37(0.029) H38(0.024)
 H40(0.018) H41(0.025) H42A(0.034) H42B(0.034) H43A(0.039) H43B(0.039)
 H44A(0.047) H44B(0.047) H45A(0.043) H45B(0.043) H46A(0.031) H46B(0.031)
 H47(0.022) H48A(0.026) H48B(0.026) H49A(0.035) H49B(0.035) H50A(0.04)
 H50B(0.04) H51A(0.038) H51B(0.038) H52A(0.032) H52B(0.032) H53(0.021)
 H54A(0.024) H54B(0.024) H55A(0.03) H55B(0.03) H56A(0.037) H56B(0.037)
 H57A(0.036) H57B(0.036) H58A(0.031) H58B(0.031) H59(0.023) H60A(0.031)
 H60B(0.031) H61A(0.04) H61B(0.04) H62A(0.04) H62B(0.04) H63A(0.037)
 H63B(0.037) H64A(0.028) H64B(0.028) H1A(0.035) H1B(0.035) H1C(0.035)
 H2A(0.031) H2B(0.031) H2C(0.031) H3A(0.037) H3B(0.037) H3C(0.037) H4A(0.035)
 H4B(0.035) H4C(0.035) H1TA(0.101) H1TB(0.101) H1TC(0.101) H7T(0.056)
 H6T(0.056) H5T(0.056) H4T(0.056) H3T(0.056) H8TA(0.15) H8TB(0.15) H8TC(0.15)
 H10T(0.114) H11T(0.114) H12T(0.114) H20T(0.114) H21T(0.114) H14C(0.15)
 H14D(0.15) H14E(0.15) H13T(0.114) H19T(0.114) H18T(0.114) H17T(0.114)
 H16T(0.114)
 Fixed X: H3(0.1071) H4(0.2336) H5(0.3225) H6(0.2846) H9(0.1079) H10A(0.2393)
 H10B(0.2403) H11A(0.3588) H11B(0.2832) H12A(0.2843) H12B(0.3093) H13A(0.1517)
 H13B(0.1519) H14A(0.0321) H14B(0.108) H15(-0.077) H16A(-0.0664) H16B(-0.1156)
 H17A(-0.2054) H17B(-0.2331) H18A(-0.3435) H18B(-0.2929) H19A(-0.2928) H19B(-
 0.2439) H20A(-0.1528) H20B(-0.1264) H21(0.3364) H22A(0.1997) H22B(0.1877)
 H23A(0.2462) H23B(0.3223) H24A(0.4031) H24B(0.3334) H25A(0.4693) H25B(0.4765)
 H26A(0.4208) H26B(0.3434) H27(0.2789) H28A(0.2951) H28B(0.3911) H29A(0.365)
 H29B(0.4328) H30A(0.5219) H30B(0.5379) H31A(0.5128) H31B(0.4154) H32A(0.4451)
 H32B(0.3797) H35(-0.2601) H36(-0.3877) H37(-0.3887) H38(-0.2671) H41(-0.165)
 H42A(-0.2745) H42B(-0.3237) H43A(-0.4111) H43B(-0.3169) H44A(-0.406) H44B(-
 0.4094) H45A(-0.2422) H45B(-0.2937) H46A(-0.1547) H46B(-0.2483) H47(0.0569)
 H48A(0.0344) H48B(-0.0124) H49A(0.1823) H49B(0.1482) H50A(0.2054) H50B(0.0961)
 H51A(0.1154) H51B(0.1606) H52A(-0.0335) H52B(-0.0005) H53(-0.1824) H54A(-
 0.3496) H54B(-0.2919) H55A(-0.4317) H55B(-0.3382) H56A(-0.4433) H56B(-0.4409)
 H57A(-0.2785) H57B(-0.3354) H58A(-0.1942) H58B(-0.2869) H59(-0.0651)
 H60A(0.0457) H60B(-0.0182) H61A(0.0773) H61B(0.1455) H62A(0.2086) H62B(0.1931)
 H63A(0.1354) H63B(0.0704) H64A(0.0407) H64B(-0.0271) H1TA(0.4897) H1TB(0.4181)
 H1TC(0.5296) H7T(0.6298) H6T(0.6529) H5T(0.5318) H4T(0.3878) H3T(0.3647)
 H8TA(0.3669) H8TB(0.4571) H8TC(0.43) H10T(0.5067) H11T(0.6082) H12T(0.6512)
 H20T(0.5928) H21T(0.4914) H14C(0.6172) H14D(0.5306) H14E(0.5292) H13T(0.4549)
 H19T(0.3721) H18T(0.3672) H17T(0.4452) H16T(0.528)
 Fixed Y: H3(0.9755) H4(1.0016) H5(0.9425) H6(0.8577) H9(0.9717) H10A(0.8999)
 H10B(0.9184) H11A(0.9614) H11B(1.0003) H12A(0.9648) H12B(1.021) H13A(1.0346)
 H13B(1.0162) H14A(0.9736) H14B(0.9343) H15(0.9091) H16A(0.984) H16B(0.956)
 H17A(0.9737) H17B(1.0016) H18A(0.936) H18B(0.9267) H19A(0.8509) H19B(0.8773)
 H20A(0.8615) H20B(0.8323) H21(0.762) H22A(0.6814) H22B(0.7332) H23A(0.6692)
 H23B(0.7139) H24A(0.6371) H24B(0.62) H25A(0.7004) H25B(0.6482) H26A(0.7138)
 H26B(0.6697) H27(0.8276) H28A(0.7546) H28B(0.7403) H29A(0.828) H29B(0.7815)
 H30A(0.8515) H30B(0.8026) H31A(0.8714) H31B(0.885) H32A(0.7961) H32B(0.8427)
 H35(0.8505) H36(0.8308) H37(0.755) H38(0.6972) H41(0.8448) H42A(0.9007)
 H42B(0.8544) H43A(0.8721) H43B(0.8662) H44A(0.792) H44B(0.7865) H45A(0.7761)
 H45B(0.7313) H46A(0.7597) H46B(0.7664) H47(0.8579) H48A(0.7755) H48B(0.7965)
 H49A(0.8116) H49B(0.7771) H50A(0.8563) H50B(0.8483) H51A(0.93) H51B(0.9082)
 H52A(0.8939) H52B(0.9289) H53(0.6277) H54A(0.6489) H54B(0.6893) H55A(0.6627)
 H55B(0.6494) H56A(0.5788) H56B(0.5793) H57A(0.5582) H57B(0.5172) H58A(0.5432)
 H58B(0.5553) H59(0.5602) H60A(0.6449) H60B(0.6116) H61A(0.5404) H61B(0.5856)
 H62A(0.5411) H62B(0.5995) H63A(0.5526) H63B(0.5193) H64A(0.6239) H64B(0.579)
 H1TA(0.4559) H1TB(0.4211) H1TC(0.4085) H7T(0.441) H6T(0.4942) H5T(0.5496)
 H4T(0.5516) H3T(0.4984) H8TA(0.4263) H8TB(0.4226) H8TC(0.4752) H10T(0.3526)
 H11T(0.3349) H12T(0.3989) H20T(0.4806) H21T(0.4982) H14C(0.5316) H14D(0.4952)
 H14E(0.5251) H13T(0.5202) H19T(0.5797) H18T(0.6638) H17T(0.6884) H16T(0.6289)
 Fixed Z: H3(0.5473) H4(0.49) H5(0.4353) H6(0.4411) H9(0.658) H10A(0.7224)
 H10B(0.6464) H11A(0.7176) H11B(0.6823) H12A(0.8175) H12B(0.7963) H13A(0.7527)
 H13B(0.8287) H14A(0.7587) H14B(0.793) H15(0.7286) H16A(0.6657) H16B(0.6006)
 H17A(0.7214) H17B(0.6516) H18A(0.6698) H18B(0.6025) H19A(0.6615) H19B(0.7278)
 H20A(0.607) H20B(0.6762) H21(0.46) H22A(0.4493) H22B(0.4084) H23A(0.3401)
 H23B(0.3508) H24A(0.3668) H24B(0.4214) H25A(0.4378) H25B(0.4779) H26A(0.5457)
 H26B(0.5352) H27(0.6217) H28A(0.6888) H28B(0.6561) H29A(0.7359) H29B(0.7582)
 H30A(0.7232) H30B(0.679) H31A(0.6071) H31B(0.6384) H32A(0.5614) H32B(0.5354)
 H35(0.4669) H36(0.5273) H37(0.5855) H38(0.5771) H41(0.2761) H42A(0.3188)
 H42B(0.3537) H43A(0.2501) H43B(0.2117) H44A(0.1974) H44B(0.2767) H45A(0.2067)
 H45B(0.243) H46A(0.31) H46B(0.349) H47(0.3918) H48A(0.3511) H48B(0.2808)
 H49A(0.333) H49B(0.2697) H50A(0.2346) H50B(0.2072) H51A(0.2507) H51B(0.3211)
 H52A(0.2672) H52B(0.3302) H53(0.3886) H54A(0.456) H54B(0.4164) H55A(0.3501)
 H55B(0.3139) H56A(0.3866) H56B(0.3068) H57A(0.3173) H57B(0.3566) H58A(0.4219)
 H58B(0.4596) H59(0.49) H60A(0.4572) H60B(0.4036) H61A(0.4292) H61B(0.4114)
 H62A(0.5087) H62B(0.5242) H63A(0.61) H63B(0.5573) H64A(0.5839) H64B(0.6039)
 H1TA(0.3468) H1TB(0.3838) H1TC(0.39) H7T(0.4714) H6T(0.5644) H5T(0.5894)
 H4T(0.5213) H3T(0.4283) H8TA(0.0531) H8TB(0.0103) H8TC(0.0425) H10T(0.0868)
 H11T(0.183) H12T(0.2601) H20T(0.2409) H21T(0.1447) H14C(0.9149) H14D(0.89)
 H14E(0.9592) H13T(0.8029) H19T(0.734) H18T(0.7681) H17T(0.871) H16T(0.9399)
;
_shelx_res_checksum              90734
_olex2_submission_special_instructions 'No special instructions were received'