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_7712020
_publ_section_title
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 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         'C27 H45 B3 P3 Sn, C16 H32 Li O4'
_chemical_formula_sum            'C43 H77 B3 Li O4 P3 Sn'
_chemical_formula_weight         909.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-12-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2022-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.1453(3)
_cell_length_b                   19.0113(2)
_cell_length_c                   30.2806(5)
_cell_measurement_reflns_used    30684
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.3270
_cell_measurement_theta_min      3.6020
_cell_volume                     9870.1(3)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.950
_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    -85.00  17.00   0.75   30.00    --   -9.14 -38.00 150.00  136
  2  \w    -23.00  88.00   0.75   30.00    --   10.16  77.00 -30.00  148
  3  \w    -19.00  83.00   0.75   30.00    --   10.16  57.00 150.00  136
  4  \w    -66.00  36.00   0.75   30.00    --   10.16 -38.00-150.00  136
  5  \w    -19.00  83.00   0.75   30.00    --   10.16  57.00  90.00  136
  6  \w     -4.00  41.00   0.75   30.00    --   10.16 -99.00 150.00   60
  7  \w      6.00  57.00   0.75   30.00    --   10.16-110.00  28.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            151804
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.809
_diffrn_reflns_theta_min         3.297
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93961
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       plate
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         12235
_refine_ls_number_restraints     1026
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+11.2647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8243
_reflns_number_total             12235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03587a2.cif
_cod_data_source_block           kji180017
_cod_depositor_comments
'Adding full bibliography for 7712014--7712020.cif.'
_cod_database_code               7712020
_shelx_shelxl_version_number     2018/3
_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 B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C37B-C36B \\sim C37A-C36A
 with sigma of 0.02
 C37B-C38B \\sim C37A-C38A
 with sigma of 0.02
 C39B-C38B \\sim C39A-C38A
 with sigma of 0.02
 O3A-C39B \\sim O3A-C39A
 with sigma of 0.02
 O3A-C36B \\sim O3A-C36A
 with sigma of 0.02
 O3B-C39B \\sim O3A-C39A
 with sigma of 0.02
 O3B-C36B \\sim O3A-C36A
 with sigma of 0.02
 O3B-Li1 \\sim O3A-Li1
 with sigma of 0.02
 O4B-C40B \\sim O4A-C40A
 with sigma of 0.02
 O4B-C43B \\sim O4A-C43A
 with sigma of 0.02
 C43B-C42B \\sim C43A-C42A
 with sigma of 0.02
 C42A-C41A \\sim C42B-C41B
 with sigma of 0.02
 C41B-C40B \\sim C41A-C40A
 with sigma of 0.02
 O4B-Li1 \\sim O4A-Li1
 with sigma of 0.02
 O2B-C32B \\sim O2A-C32A
 with sigma of 0.02
 C33B-C32B \\sim C33A-C32A
 with sigma of 0.02
 C34B-C33B \\sim C34A-C33A
 with sigma of 0.02
 C35A-C34A \\sim C35B-C34B
 with sigma of 0.02
 O2A-C35A \\sim O2B-C35B
 with sigma of 0.02
 O2A-Li1 \\sim O2B-Li1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O3A \\sim C36A \\sim C37A \\sim C38A \\sim C39A \\sim O3B \\sim C36B \\sim C37B
\\sim C38B \\sim C39B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O2A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim O2B \\sim C32B \\sim C33B
\\sim C34B \\sim C35B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O4A \\sim C40A \\sim C41A \\sim C42A \\sim C43A \\sim O4B \\sim C40B \\sim C41B
\\sim C42B \\sim C43B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
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. Others
 Fixed Sof: O2A(0.71974) O3A(0.57918) O4A(0.67672) C32A(0.71974) H32A(0.71974)
 H32B(0.71974) C33A(0.71974) H33A(0.71974) H33B(0.71974) C34A(0.71974)
 H34A(0.71974) H34B(0.71974) C35A(0.71974) H35A(0.71974) H35B(0.71974)
 C36A(0.57918) H36A(0.57918) H36B(0.57918) C37A(0.57918) H37A(0.57918)
 H37B(0.57918) C38A(0.57918) H38A(0.57918) H38B(0.57918) C39A(0.57918)
 H39A(0.57918) H39B(0.57918) C40A(0.67672) H40A(0.67672) H40B(0.67672)
 C41A(0.67672) H41A(0.67672) H41B(0.67672) C42A(0.67672) H42A(0.67672)
 H42B(0.67672) C43A(0.67672) H43A(0.67672) H43B(0.67672) O2B(0.28026)
 O3B(0.42082) O4B(0.32328) C32B(0.28026) H32C(0.28026) H32D(0.28026)
 C33B(0.28026) H33C(0.28026) H33D(0.28026) C34B(0.28026) H34C(0.28026)
 H34D(0.28026) C35B(0.28026) H35C(0.28026) H35D(0.28026) C36B(0.42082)
 H36C(0.42082) H36D(0.42082) C37B(0.42082) H37C(0.42082) H37D(0.42082)
 C38B(0.42082) H38C(0.42082) H38D(0.42082) C39B(0.42082) H39C(0.42082)
 H39D(0.42082) C40B(0.32328) H40C(0.32328) H40D(0.32328) C41B(0.32328)
 H41C(0.32328) H41D(0.32328) C42B(0.32328) H42C(0.32328) H42D(0.32328)
 C43B(0.32328) H43C(0.32328) H43D(0.32328)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C16(H16), C25(H25)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32A(H32A,
 H32B), C33A(H33A,H33B), C34A(H34A,H34B), C35A(H35A,H35B), C36A(H36A,H36B),
 C37A(H37A,H37B), C38A(H38A,H38B), C39A(H39A,H39B), C40A(H40A,H40B), C41A(H41A,
 H41B), C42A(H42A,H42B), C43A(H43A,H43B), C32B(H32C,H32D), C33B(H33C,H33D),
 C34B(H34C,H34D), C35B(H35C,H35D), C36B(H36C,H36D), C37B(H37C,H37D), C38B(H38C,
 H38D), C39B(H39C,H39D), C40B(H40C,H40D), C41B(H41C,H41D), C42B(H42C,H42D),
 C43B(H43C,H43D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              20029
_shelx_hkl_checksum              81985
_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
;