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_7712018
_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         '1(C44 H57 B3 Na O2 P3 Sn)'
_chemical_formula_sum            'C44 H57 B3 Na O2 P3 Sn'
_chemical_formula_weight         884.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-19
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:34:44 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2022-11-04 deposited with the CCDC.	2022-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                113.1030(19)
_cell_angle_beta                 93.1405(17)
_cell_angle_gamma                91.4023(16)
_cell_formula_units_Z            4
_cell_length_a                   12.1003(2)
_cell_length_b                   19.4551(4)
_cell_length_c                   21.1123(4)
_cell_measurement_reflns_used    24299
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.4530
_cell_measurement_theta_min      3.4880
_cell_volume                     4558.92(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -19.00  84.00   1.00   14.00    --   10.16  57.00 -90.00  103
  2  \w    -23.00  89.00   1.00   14.00    --   10.16  77.00 120.00  112
  3  \w    -66.00  37.00   1.00   14.00    --   10.16 -38.00  30.00  103
  4  \w    -69.00  44.00   1.00   14.00    --   10.16 -77.00   0.00  113
  5  \w    -39.00  65.00   1.00   14.00    --   -9.14  57.00-180.00  104
  6  \w    -16.00  62.00   1.00   14.00    --   10.16  38.00  30.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0406499000
_diffrn_orient_matrix_UB_12      -0.0203947000
_diffrn_orient_matrix_UB_13      0.0096649000
_diffrn_orient_matrix_UB_21      -0.0308538000
_diffrn_orient_matrix_UB_22      0.0014992000
_diffrn_orient_matrix_UB_23      0.0280881000
_diffrn_orient_matrix_UB_31      -0.0291676000
_diffrn_orient_matrix_UB_32      -0.0340125000
_diffrn_orient_matrix_UB_33      -0.0214092000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            73117
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.836
_diffrn_reflns_theta_min         3.226
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
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    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1176
_refine_ls_number_reflns         20675
_refine_ls_number_restraints     1674
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+1.3765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15100
_reflns_number_total             20675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03587a2.cif
_cod_data_source_block           kji170030
_cod_depositor_comments
'Adding full bibliography for 7712014--7712020.cif.'
_cod_original_cell_volume        4558.93(17)
_cod_database_code               7712018
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C36 H39 B3 P3 Sn1'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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 B(H) groups, All B(H,H) groups, All C(H,H,H) groups, All C(H,H,H,H,H,H,
  H,H,H,H) groups
2. Restrained distances
 O2-C77A \\sim O2-C77B
 with sigma of 0.02
 C78B-C77B \\sim C78A-C77A
 with sigma of 0.02
 O2-C78A \\sim O2-C78B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C73A \\sim C74A \\sim C75A \\sim C76A \\sim C73B \\sim C74B \\sim C75B
\\sim C76B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O3A \\sim C81A \\sim C82A \\sim C83A \\sim C84A \\sim O3B \\sim C81B \\sim C82B
\\sim C83B \\sim C84B \\sim O3C \\sim C81C \\sim C82C \\sim C83C \\sim C84C:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C77A \\sim C77B \\sim C78A \\sim C78B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O3B, C81B, C82B, C83B, C84B} sigma for 1-2: 0.02, 1-3: 0.02
{O3C, C81C, C82C, C83C, C84C} sigma for 1-2: 0.02, 1-3: 0.02
{O1, C73A, C74A, C75A, C76A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O3A, C81A, C82A, C83A, C84A}
{C73A, C74A, C75A, C76A} sigma for 1-2: 0.02, 1-3: 0.02
as
{C73B, C74B, C75B, C76B}
6. Others
 Fixed Sof: C73A(0.53551) H73A(0.53551) H73B(0.53551) C74A(0.53551)
 H74A(0.53551) H74B(0.53551) C75A(0.53551) H75A(0.53551) H75B(0.53551)
 C76A(0.53551) H76A(0.53551) H76B(0.53551) O3A(0.32528) C81A(0.32528)
 H81A(0.32528) H81B(0.32528) C82A(0.32528) H82A(0.32528) H82B(0.32528)
 C83A(0.32528) H83A(0.32528) H83B(0.32528) C84A(0.32528) H84A(0.32528)
 H84B(0.32528) C73B(0.46449) H73C(0.46449) H73D(0.46449) C74B(0.46449)
 H74C(0.46449) H74D(0.46449) C75B(0.46449) H75C(0.46449) H75D(0.46449)
 C76B(0.46449) H76C(0.46449) H76D(0.46449) C77A(0.79093) H77A(0.79093)
 H77B(0.79093) C78A(0.79093) H78A(0.79093) H78B(0.79093) H78C(0.79093)
 O3B(0.44225) C81B(0.44225) H81C(0.44225) H81D(0.44225) C82B(0.44225)
 H82C(0.44225) H82D(0.44225) C83B(0.44225) H83C(0.44225) H83D(0.44225)
 C84B(0.44225) H84C(0.44225) H84D(0.44225) C77B(0.20907) H77C(0.20907)
 H77D(0.20907) C78B(0.20907) H78D(0.20907) H78E(0.20907) H78F(0.20907)
 O3C(0.23206) C81C(0.23206) H81E(0.23206) H81F(0.23206) C82C(0.23206)
 H82E(0.23206) H82F(0.23206) C83C(0.23206) H83E(0.23206) H83F(0.23206)
 C84C(0.23206) H84E(0.23206) H84F(0.23206)
7.a Secondary CH2 refined with riding coordinates:
 C73A(H73A,H73B), C74A(H74A,H74B), C75A(H75A,H75B), C76A(H76A,H76B), C79(H79A,
 H79B), C85(H85A,H85B), C87(H87A,H87B), C81A(H81A,H81B), C82A(H82A,H82B),
 C83A(H83A,H83B), C84A(H84A,H84B), C73B(H73C,H73D), C74B(H74C,H74D), C75B(H75C,
 H75D), C76B(H76C,H76D), C77A(H77A,H77B), C81B(H81C,H81D), C82B(H82C,H82D),
 C83B(H83C,H83D), C84B(H84C,H84D), C77B(H77C,H77D), C81C(H81E,H81F), C82C(H82E,
 H82F), C83C(H83E,H83F), C84C(H84E,H84F)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), 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), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
7.c Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C86(H86A,H86B,H86C), C88(H88A,H88B,H88C), C78A(H78A,H78B,
 H78C), C78B(H78D,H78E,H78F)
;
_shelx_res_checksum              88733
_shelx_hkl_checksum              9420
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.050
_oxdiff_exptl_absorpt_empirical_full_min 0.977