Phosphido-borane-supported stannates.
Izod, Keith; Madlool, Atheer M.; Craig, Alex; Waddell, Paul G.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 947–954; doi:10.1039/d2dt03587a

data_7712016
_publ_section_title
;
 Phosphido-borane-supported stannates.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              947
_journal_page_last               954
_journal_paper_doi               10.1039/d2dt03587a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C30 H75 B3 Li O3 P3 Sn'
_chemical_formula_sum            'C30 H75 B3 Li O3 P3 Sn'
_chemical_formula_weight         734.87
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2022-11-04 deposited with the CCDC.	2022-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.9907(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.40488(9)
_cell_length_b                   20.31668(13)
_cell_length_c                   17.70719(13)
_cell_measurement_reflns_used    15356
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.7710
_cell_measurement_theta_min      3.4100
_cell_volume                     4193.79(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -34.00    5.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905   19.0000 -180.0000 39

  2 omega  -25.00   56.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905  -77.0000 -150.0000 81

  3 omega   -3.00   67.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905 -125.0000   90.0000 70

  4 omega   20.00   77.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   60.0000 57

  5 omega   49.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  150.0000 26

  6 omega   22.00   96.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   90.0000 74

  7 omega   74.00  162.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000  -30.0000 88

  8 omega  132.00  167.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000   60.0000 35

  9 omega   53.00   80.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -180.0000 27

 10 omega   30.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  -90.0000 39

 11 omega   22.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -150.0000 102

 12 omega   30.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000 -120.0000 39

 13 omega   24.00   50.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000    0.0000 26

 14 omega   79.00  109.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000    0.0000 30

 15 omega   83.00  118.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000   60.0000 35

 16 omega   17.00   55.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -60.0000 38

 17 omega   27.00   76.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  120.0000 49

 18 omega   89.00  156.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000   60.0000 67

 19 omega   93.00  119.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -150.0000 26

 20 omega  124.00  150.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -150.0000 26

 21 omega   31.00   57.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  120.0000 26

 22 omega   12.00   84.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   57.0000    0.0000 72

 23 omega   12.00  116.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   57.0000  150.0000 104
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0312575000
_diffrn_orient_matrix_UB_12      0.0624326000
_diffrn_orient_matrix_UB_13      0.0524337000
_diffrn_orient_matrix_UB_21      0.0961363000
_diffrn_orient_matrix_UB_22      0.0153136000
_diffrn_orient_matrix_UB_23      -0.0340220000
_diffrn_orient_matrix_UB_31      -0.0850148000
_diffrn_orient_matrix_UB_32      0.0402474000
_diffrn_orient_matrix_UB_33      -0.0683113000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30391
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.962
_diffrn_reflns_theta_min         3.433
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.107
_exptl_absorpt_correction_T_max  0.637
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7442
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0309P)^2^+0.8992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6441
_reflns_number_total             7442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03587a2.cif
_cod_data_source_block           kji150020_fa
_cod_depositor_comments
'Adding full bibliography for 7712014--7712020.cif.'
_cod_original_cell_volume        4193.79(5)
_cod_database_code               7712016
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C30 H76 B3 Li1 O3 P3 Sn1'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C19B \\sim O1-C19A
 with sigma of 0.02
 O1-C22A \\sim O1-C22B
 with sigma of 0.02
 C21B-C22B \\sim C22A-C21A
 with sigma of 0.02
 C20A-C21A \\sim C21B-C20B
 with sigma of 0.02
 C19A-C20A \\sim C20B-C19B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C19B) = Uanis(C19A)
Uanis(C20B) = Uanis(C20A)
Uanis(C21B) = Uanis(C21A)
Uanis(C22B) = Uanis(C22A)
4. Rigid body (RIGU) restrains
 C19B, C22B, C19A, C22A, C20B, C21B, C20A, C21A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C19B(0.49775) H19A(0.49775) H19B(0.49775) C20B(0.49775)
 H20A(0.49775) H20B(0.49775) C21B(0.49775) H21A(0.49775) H21B(0.49775)
 C22B(0.49775) H22A(0.49775) H22B(0.49775) C19A(0.50225) H19C(0.50225)
 H19D(0.50225) C20A(0.50225) H20C(0.50225) H20D(0.50225) C21A(0.50225)
 H21C(0.50225) H21D(0.50225) C22A(0.50225) H22C(0.50225) H22D(0.50225)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C19B(H19A,H19B),
 C20B(H20A,H20B), C21B(H21A,H21B), C22B(H22A,H22B), C19A(H19C,H19D), C20A(H20C,
 H20D), C21A(H21C,H21D), C22A(H22C,H22D)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              36422
_shelx_hkl_checksum              24424
_olex2_submission_special_instructions 'No special instructions were received'