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_1550502
_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         'C58 H72 Na2 O14 P2, C4 H8 O'
_chemical_formula_sum            'C62 H80 Na2 O15 P2'
_chemical_formula_weight         1173.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.726(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5839(10)
_cell_length_b                   9.1559(2)
_cell_length_c                   28.1190(11)
_cell_measurement_reflns_used    7737
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.4410
_cell_measurement_theta_min      3.6240
_cell_volume                     6040.4(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega -114.00  -14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038  -57.0000   30.0000 100

  2 omega  -71.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038   77.0000  150.0000 106

  3 omega   -6.00   79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7038  -93.0000  -69.0000 85

  4 omega   34.00   95.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -45.0000   30.0000 61

  5 omega   41.00   86.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -30.0000  120.0000 45

  6 omega   38.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -95.0000  -90.0000 71

  7 omega   92.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326   30.0000 -180.0000 85

  8 omega   60.00  170.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326   15.0000  -60.0000 110

  9 omega  110.00  170.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  125.0000  120.0000 60

 10 omega   37.00  137.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -77.0000  120.0000 100

 11 omega   26.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -95.0000   60.0000 83

 12 omega   34.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -45.0000 -120.0000 64
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0426422000
_diffrn_orient_matrix_UB_12      -0.0634375000
_diffrn_orient_matrix_UB_13      -0.0142397000
_diffrn_orient_matrix_UB_21      0.0478665000
_diffrn_orient_matrix_UB_22      0.0096717000
_diffrn_orient_matrix_UB_23      0.0620853000
_diffrn_orient_matrix_UB_31      -0.0143109000
_diffrn_orient_matrix_UB_32      -0.1554907000
_diffrn_orient_matrix_UB_33      0.0096466000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17565
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.905
_diffrn_reflns_theta_min         3.635
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0496P)^2^+5.6347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1015
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5196
_reflns_number_total             6005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05281f2.cif
_cod_data_source_block           exp_1709
_cod_original_cell_volume        6040.4(4)
_cod_database_code               1550502
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O P Na'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: O2(0.5) C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5)
3.a Free rotating group:
 O2(C31,C32,C33,C34)
3.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C19(H19A,H19B), C22(H22A,H22B), C30(H30A,H30B), C20(H20A,
 H20B), C23(H23A,H23B), C29(H29A,H29B), C27(H27A,H27B), C25(H25A,H25B),
 C21(H21A,H21B), C26(H26A,H26B), C28(H28A,H28B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C17(H17), C13(H13), C14(H14), C15(H15), C16(H16), C7(H7),
 C11(H11), C8(H8), C10(H10), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'