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_1550500
_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         'C40 H60 Cl2 Cu2 O4 P4'
_chemical_formula_sum            'C40 H60 Cl2 Cu2 O4 P4'
_chemical_formula_weight         926.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                79.859(5)
_cell_angle_beta                 71.565(6)
_cell_angle_gamma                66.823(7)
_cell_formula_units_Z            1
_cell_length_a                   9.1382(8)
_cell_length_b                   11.4943(8)
_cell_length_c                   12.1632(7)
_cell_measurement_reflns_used    3370
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.1790
_cell_measurement_theta_min      5.4580
_cell_volume                     1112.26(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.953
_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    -65.00  27.00   1.00    2.00    --  -41.14  38.00  30.00   92
  2  \w    -73.00  24.00   1.00    2.00    --  -41.14  77.00 120.00   97
  3  \w    100.00 128.00   1.00    2.00    --   41.14 178.00   0.00   28
  4  \w    101.00 176.00   1.00    7.00    --  106.40 125.00 -90.00   75
  5  \w    144.00 171.00   1.00    7.00    --  106.40  77.00-150.00   27
  6  \w     82.00 169.00   1.00    7.00    --  106.40  45.00 -30.00   87
  7  \w     82.00 135.00   1.00    7.00    --  106.40 -61.00-120.00   53
  8  \w     77.00 109.00   1.00    7.00    --  106.40 -95.00 -90.00   32
  9  \w     48.00 114.00   1.00    7.00    --  106.40 -77.00   0.00   66
 10  \w     47.00  78.00   1.00    7.00    --  106.40 -61.00-120.00   31
 11  \w     24.00  55.00   1.00    7.00    --  106.40 -95.00 -90.00   31
 12  \w     29.00  98.00   1.00    7.00    --  106.40 -95.00-150.00   69
 13  \w     76.00 112.00   1.00    7.00    --  106.40  77.00-150.00   36
 14  \w     56.00 173.00   1.00    7.00    --  106.40  15.00  90.00  117
 15  \w     93.00 120.00   1.00    7.00    --  106.40-125.00 150.00   27
 16  \w     38.00  64.00   1.00    7.00    --  106.40-125.00 150.00   26
 17  \w   -113.00 -17.00   1.00    2.00    --  -41.14 -38.00-150.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1628292000
_diffrn_orient_matrix_UB_12      -0.0161773000
_diffrn_orient_matrix_UB_13      0.0240958000
_diffrn_orient_matrix_UB_21      0.0895419000
_diffrn_orient_matrix_UB_22      -0.0145625000
_diffrn_orient_matrix_UB_23      -0.1302559000
_diffrn_orient_matrix_UB_31      -0.0424817000
_diffrn_orient_matrix_UB_32      0.1444193000
_diffrn_orient_matrix_UB_33      -0.0184386000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6787
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.772
_diffrn_reflns_theta_min         3.838
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0850P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3704
_reflns_number_total             4298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05281f2.cif
_cod_data_source_block           exp_1726_a
_cod_original_cell_volume        1112.26(16)
_cod_database_code               1550500
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.538
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C2(H2A), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C10(H10A,H10B,H10C)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1)
;
_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 2.493
_oxdiff_exptl_absorpt_empirical_full_min 0.519