Making the Unconventional μ2-P Bridging Binding Mode More Conventional in Phosphinine Complexes
Gruetzmacher, Hansjoerg; Hou, Yuanfeng; Li, Zhongshu; Li, Yaqi; Su, Cheng-Yong; Puschmann, Florian; Liu, Peng; Chemical Science  (2019) –; doi:10.1039/C8SC05281F

data_1550495
_publ_section_title
;
 Making the Unconventional \m2-P Bridging Binding Mode More Conventional
 in Phosphinine Complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05281F
_journal_year                    2019
_chemical_formula_moiety         'C35 H27 O P Sn'
_chemical_formula_sum            'C35 H27 O P Sn'
_chemical_formula_weight         613.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.801(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.93270(10)
_cell_length_b                   18.4467(3)
_cell_length_c                   15.8535(2)
_cell_measurement_reflns_used    6399
_cell_measurement_temperature    149.93(15)
_cell_measurement_theta_max      74.1950
_cell_measurement_theta_min      3.7330
_cell_volume                     2808.38(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.93(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_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    -66.00  26.00   1.00    1.00    --  -41.14  38.00-120.00   92
  2  \w   -113.00 -20.00   1.00    1.00    --  -41.14 -38.00  60.00   93
  3  \w     61.00 100.00   1.00    1.00    --   41.14 178.00   0.00   39
  4  \w     83.00 109.00   1.00    1.50    --  107.98  45.00  60.00   26
  5  \w     32.00 132.00   1.00    1.50    --  107.98 -30.00-120.00  100
  6  \w     36.00 123.00   1.00    1.50    --  107.98 -45.00  30.00   87
  7  \w     38.00  74.00   1.00    1.50    --  107.98 -95.00  30.00   36
  8  \w     99.00 138.00   1.00    1.50    --  107.98 125.00 -60.00   39
  9  \w    129.00 171.00   1.00    1.50    --  107.98  45.00  60.00   42
 10  \w     95.00 156.00   1.00    1.50    --  107.98  45.00 120.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1557678000
_diffrn_orient_matrix_UB_12      0.0186375000
_diffrn_orient_matrix_UB_13      0.0164539000
_diffrn_orient_matrix_UB_21      0.0182335000
_diffrn_orient_matrix_UB_22      -0.0626051000
_diffrn_orient_matrix_UB_23      -0.0604669000
_diffrn_orient_matrix_UB_31      -0.0338452000
_diffrn_orient_matrix_UB_32      0.0520542000
_diffrn_orient_matrix_UB_33      -0.0785526000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10059
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.095
_diffrn_reflns_theta_min         3.749
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0550P)^2^+0.5750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5242
_reflns_number_total             5500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05281f2.cif
_cod_data_source_block           exp_2558
_cod_database_code               1550495
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.448
_shelx_estimated_absorpt_t_min   0.381
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C24(H24), C23(H23), C28(H28), C13(H13), C35(H35), C31(H31),
 C16(H16), C34(H34), C33(H33), C14(H14), C17(H17), C7(H7), C19(H19), C11(H11),
 C15(H15), C32(H32), C25(H25), C27(H27), C22(H22), C26(H26), C10(H10), C8(H8),
 C21(H21), C20(H20), C9(H9)
;
_olex2_date_sample_data_collection 2018-03-20
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.886
_oxdiff_exptl_absorpt_empirical_full_min 0.759