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_7712019
_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         'C22 H61 B3 K O P3 Sn'
_chemical_formula_sum            'C22 H61 B3 K O P3 Sn'
_chemical_formula_weight         624.83
_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     dual
_audit_creation_date             2017-10-24
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2022-11-04 deposited with the CCDC.	2022-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5136(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.09083(13)
_cell_length_b                   15.64326(17)
_cell_length_c                   20.3678(3)
_cell_measurement_reflns_used    42904
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      29.0640
_cell_measurement_theta_min      3.6630
_cell_volume                     3517.40(8)
_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 0.925
_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    -70.00  -1.00   1.00   10.00    --   -9.14 130.00-119.70   69
  2  \w    -16.00  86.00   1.00   10.00    --   10.16  38.00 150.00  102
  3  \w    -16.00  86.00   1.00   10.00    --   10.16  38.00-120.00  102
  4  \w    -19.00  84.00   1.00   10.00    --   10.16  57.00 -60.00  103
  5  \w    -36.00  92.00   1.00   10.00    --   10.16  19.00  90.00  128
  6  \w    -65.00  45.00   1.00   10.00    --   12.00 -72.00 101.41  110
  7  \w    -11.00  52.00   1.00   10.00    --   12.00 -93.00  32.18   63
  8  \w     22.00  72.00   1.00   10.00    --   12.00-129.00-117.01   50
  9  \w    -31.00  26.00   1.00   10.00    --   10.16  98.00  27.00   57
 10  \w    -23.00  89.00   1.00   10.00    --   10.16  77.00 150.00  112
 11  \w     -4.00  52.00   1.00   10.00    --   10.16 -99.00 -60.00   56
 12  \w    -36.00  92.00   1.00   10.00    --   10.16  19.00 -90.00  128
 13  \w     22.00  74.00   1.00   10.00    --   12.00-132.00-131.75   52
 14  \w    -12.00  51.00   1.00   10.00    --   12.00 -92.00  87.94   63
 15  \w    -16.00  23.00   1.00   10.00    --   10.16  38.00 120.00   39
;
_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      -0.0156408000
_diffrn_orient_matrix_UB_12      -0.0229076000
_diffrn_orient_matrix_UB_13      -0.0296648000
_diffrn_orient_matrix_UB_21      0.0269175000
_diffrn_orient_matrix_UB_22      -0.0373928000
_diffrn_orient_matrix_UB_23      0.0146419000
_diffrn_orient_matrix_UB_31      -0.0561878000
_diffrn_orient_matrix_UB_32      -0.0115488000
_diffrn_orient_matrix_UB_33      0.0114064000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            112187
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.500
_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    0.993
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.802
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         9067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0148P)^2^+1.2742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7542
_reflns_number_total             9067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03587a2.cif
_cod_data_source_block           kji170055_fa
_cod_depositor_comments
'Adding full bibliography for 7712014--7712020.cif.'
_cod_original_cell_volume        3517.40(7)
_cod_database_code               7712019
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C23 H61 B3 K1 O1 P3 Sn1'
_reflns_odcompleteness_completeness 99.72
_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.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B)
2.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),
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              12557
_shelx_hkl_checksum              51053
_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 1.018
_oxdiff_exptl_absorpt_empirical_full_min 0.968