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_7712014
_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_absolute_configuration ad
_chemical_formula_moiety         'C40 H47 B3 Li O P3 Sn'
_chemical_formula_sum            'C40 H47 B3 Li O P3 Sn'
_chemical_formula_weight         794.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-20
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0937(3)
_cell_length_b                   17.3507(5)
_cell_length_c                   19.0102(6)
_cell_measurement_reflns_used    7430
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      27.2890
_cell_measurement_theta_min      3.1750
_cell_volume                     3989.0(2)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -43.00  70.00   1.00   15.00    --   -9.06  77.00-180.00  113
  2  \w      3.00  59.00   1.00   15.00    --   -9.06  77.00 -90.00   56
  3  \w     -4.00  21.00   1.00   15.00    --   10.00 -99.00  90.00   25
  4  \w    -54.00 -28.00   1.00   15.00    --   10.16 -19.00 -30.00   26
;
_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      0.0155860000
_diffrn_orient_matrix_UB_12      0.0330552000
_diffrn_orient_matrix_UB_13      0.0195948000
_diffrn_orient_matrix_UB_21      0.0544795000
_diffrn_orient_matrix_UB_22      -0.0147242000
_diffrn_orient_matrix_UB_23      0.0031316000
_diffrn_orient_matrix_UB_31      0.0150531000
_diffrn_orient_matrix_UB_32      0.0190140000
_diffrn_orient_matrix_UB_33      -0.0316150000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21477
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.890
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
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)
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    1.323
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 2462 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.047(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         7674
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0232P)^2^+0.6750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.957
_reflns_number_gt                6394
_reflns_number_total             7674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03587a2.cif
_cod_data_source_block           kji160027_fa
_cod_depositor_comments
'Adding full bibliography for 7712014--7712020.cif.'
_cod_original_cell_volume        3988.99(19)
_cod_database_code               7712014
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C40 H47 B3 Li1 O1 P3 Sn1'
_reflns_odcompleteness_completeness 99.71
_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,H,H) groups
2. Restrained distances
 O1A-Li1 \\sim O1B-Li1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1A) = Uanis(O1B)
Uanis(C37A) = Uanis(C37B)
Uanis(C38A) = Uanis(C38B)
Uanis(C39A) = Uanis(C39B)
Uanis(C40A) = Uanis(C40B)
4. Rigid body (RIGU) restrains
 O1A, C37A, C38A, C39A, C40A, O1B, C37B, C38B, C39B, C40B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O1A, C37A, C38A, C39A, C40A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O1B, C37B, C38B, C39B, C40B}
6. Others
 Fixed Sof: O1A(0.49087) C37A(0.49087) H37A(0.49087) H37B(0.49087)
 C38A(0.49087) H38A(0.49087) H38B(0.49087) C39A(0.49087) H39A(0.49087)
 H39B(0.49087) C40A(0.49087) H40A(0.49087) H40B(0.49087) O1B(0.50913)
 C37B(0.50913) H37C(0.50913) H37D(0.50913) C38B(0.50913) H38C(0.50913)
 H38D(0.50913) C39B(0.50913) H39C(0.50913) H39D(0.50913) C40B(0.50913)
 H40C(0.50913) H40D(0.50913)
7.a Secondary CH2 refined with riding coordinates:
 C37A(H37A,H37B), C38A(H38A,H38B), C39A(H39A,H39B), C40A(H40A,H40B), C37B(H37C,
 H37D), C38B(H38C,H38D), C39B(H39C,H39D), C40B(H40C,H40D)
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)
;
_shelx_res_checksum              19713
_shelx_hkl_checksum              1934
_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 1.020
_oxdiff_exptl_absorpt_empirical_full_min 0.973