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_7712017
_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         'C88 H114 B6 K2 O4 P6 Sn2'
_chemical_formula_sum            'C88 H114 B6 K2 O4 P6 Sn2'
_chemical_formula_weight         1802.05
_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             2017-06-30
_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                83.991(3)
_cell_angle_beta                 75.367(3)
_cell_angle_gamma                62.619(4)
_cell_formula_units_Z            1
_cell_length_a                   12.5263(4)
_cell_length_b                   12.8410(6)
_cell_length_c                   16.3428(5)
_cell_measurement_reflns_used    11581
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      26.9530
_cell_measurement_theta_min      3.5340
_cell_volume                     2258.32(17)
_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      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 0.998
_diffrn_measured_fraction_theta_max 0.862
_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     -4.00  52.00   1.00   45.00    --   10.16 -99.00 -30.00   56
  2  \w     31.00  78.00   1.00   45.00    --   10.16-144.00 149.00   47
  3  \w    -71.00  56.00   1.00   45.00    --   10.16 -19.00 150.00  127
  4  \w    -36.00  92.00   1.00   45.00    --   10.16  19.00 -30.00  128
  5  \w    -58.00 -10.00   1.00   45.00    --   10.16 144.00-156.00   48
  6  \w    -66.00  37.00   1.00   45.00    --   10.16 -38.00   0.00  103
  7  \w    -16.00  86.00   1.00   45.00    --   10.16  38.00-180.00  102
;
_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      -0.0123752000
_diffrn_orient_matrix_UB_12      -0.0042729000
_diffrn_orient_matrix_UB_13      0.0447083000
_diffrn_orient_matrix_UB_21      -0.0169009000
_diffrn_orient_matrix_UB_22      -0.0450551000
_diffrn_orient_matrix_UB_23      -0.0024825000
_diffrn_orient_matrix_UB_31      0.0621134000
_diffrn_orient_matrix_UB_32      -0.0426861000
_diffrn_orient_matrix_UB_33      -0.0027299000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36224
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.831
_diffrn_reflns_theta_min         3.284
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99641
_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    1.325
_exptl_crystal_description       plate
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         10194
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0331P)^2^+0.5192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7863
_reflns_number_total             10194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03587a2.cif
_cod_data_source_block           kji170036
_cod_depositor_comments
'Adding full bibliography for 7712014--7712020.cif.'
_cod_original_cell_volume        2258.33(16)
_cod_database_code               7712017
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C36 H39 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,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 K1-O2B \\sim K1-O2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2A \\sim C41A \\sim C42A \\sim C43A \\sim C44A \\sim O2B \\sim C41B \\sim C42B
\\sim C43B \\sim C44B: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
4. Rigid body (RIGU) restrains
 O2A, C41A, C42A, C43A, C44A, O2B, C41B, C42B, C43B, C44B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O2A, C41A, C42A, C43A, C44A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O2B, C41B, C42B, C43B, C44B}
6. Others
 Fixed Sof: O2A(0.65416) C41A(0.65416) H41A(0.65416) H41B(0.65416)
 C42A(0.65416) H42A(0.65416) H42B(0.65416) H42C(0.65416) C43A(0.65416)
 H43A(0.65416) H43B(0.65416) C44A(0.65416) H44A(0.65416) H44B(0.65416)
 H44C(0.65416) O2B(0.34584) C41B(0.34584) H41C(0.34584) H41D(0.34584)
 C42B(0.34584) H42D(0.34584) H42E(0.34584) H42F(0.34584) C43B(0.34584)
 H43C(0.34584) H43D(0.34584) C44B(0.34584) H44D(0.34584) H44E(0.34584)
 H44F(0.34584)
7.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41A(H41A,
 H41B), C43A(H43A,H43B), C41B(H41C,H41D), C43B(H43C,H43D)
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)
7.c Idealised Me refined as rotating group:
 C42A(H42A,H42B,H42C), C44A(H44A,H44B,H44C), C42B(H42D,H42E,H42F), C44B(H44D,
 H44E,H44F)
;
_shelx_res_checksum              21567
_shelx_hkl_checksum              17982
_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 1.034
_oxdiff_exptl_absorpt_empirical_full_min 0.969