#------------------------------------------------------------------------------
#$Date: 2019-01-22 01:19:44 +0200 (Tue, 22 Jan 2019) $
#$Revision: 213240 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/05/1550501.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1550501
loop_
_publ_author_name
'Gruetzmacher, Hansjoerg'
'Hou, Yuanfeng'
'Li, Zhongshu'
'Li, Yaqi'
'Su, Cheng-Yong'
'Puschmann, Florian'
'Liu, Peng'
_publ_section_title
;
 Making the Unconventional μ2-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         'C28 H36 Cl2 Cu2 O4 P4'
_chemical_formula_sum            'C28 H36 Cl2 Cu2 O4 P4'
_chemical_formula_weight         758.43
_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
_atom_sites_solution_primary     dual
_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                78.259(4)
_cell_angle_beta                 87.754(4)
_cell_angle_gamma                80.431(4)
_cell_formula_units_Z            1
_cell_length_a                   8.0889(4)
_cell_length_b                   9.7187(5)
_cell_length_c                   10.6284(5)
_cell_measurement_reflns_used    3088
_cell_measurement_temperature    290.85(10)
_cell_measurement_theta_max      72.8260
_cell_measurement_theta_min      5.5380
_cell_volume                     806.66(7)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.85(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  27.00   1.00    1.00    --  -41.14  57.00  60.00   93
  2  ω   -106.00 -13.00   1.00    1.00    --  -41.14 -57.00 -90.00   93
  3  ω   -130.00 -37.00   1.00    1.00    --  -41.14-178.00  60.00   93
  4  ω     79.00 121.00   1.00    1.00    --  106.40-125.00 150.00   42
  5  ω     46.00  72.00   1.00    1.00    --  106.40-125.00 150.00   26
  6  ω     33.00 139.00   1.00    1.00    --  106.40 -77.00 -60.00  106
  7  ω     81.00 165.00   1.00    1.00    --  106.40  45.00  30.00   84
  8  ω     96.00 177.00   1.00    1.00    --  106.40 125.00 -90.00   81
  9  ω     96.00 148.00   1.00    1.00    --  106.40 125.00  30.00   52
 10  ω     86.00 178.00   1.00    1.00    --  106.40  61.00 -30.00   92
 11  ω     77.00 157.00   1.00    1.00    --  106.40  61.00  90.00   80
 12  ω     30.00 107.00   1.00    1.00    --  106.40 -95.00-120.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0305249000
_diffrn_orient_matrix_UB_12      0.1363478000
_diffrn_orient_matrix_UB_13      0.0560807000
_diffrn_orient_matrix_UB_21      -0.0175996000
_diffrn_orient_matrix_UB_22      0.0911829000
_diffrn_orient_matrix_UB_23      -0.1369395000
_diffrn_orient_matrix_UB_31      -0.1899021000
_diffrn_orient_matrix_UB_32      -0.0033749000
_diffrn_orient_matrix_UB_33      0.0045130000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4593
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.247
_diffrn_reflns_theta_min         4.249
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10003
_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    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0941P)²+1.1527P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2904
_reflns_number_total             3062
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc05281f2.cif
_cod_data_source_block           exp_1748
_cod_database_code               1550501
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.504
_shelx_estimated_absorpt_t_min   0.403
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C2(H2A), C9(H9), C4(H4)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C7(H7A,H7B,H7C)
2.c 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 4.635
_oxdiff_exptl_absorpt_empirical_full_min 0.527
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Cu1 Cu 0.86334(6) 0.46080(5) 0.56516(5) 0.0199(2) Uani 1 1 d .
Cl1 Cl 0.91324(11) 0.26179(9) 0.73255(8) 0.0237(2) Uani 1 1 d .
P1 P 0.62434(11) 0.58658(9) 0.62540(8) 0.0197(2) Uani 1 1 d .
P2 P 0.94076(11) 0.37371(9) 0.38812(8) 0.0182(2) Uani 1 1 d .
O2 O 1.1167(3) 0.1315(3) 0.5238(3) 0.0273(6) Uani 1 1 d .
H2 H 1.0561 0.1627 0.5812 0.041 Uiso 1 1 calc GR
O1 O 0.6785(4) 0.4672(3) 0.8764(3) 0.0324(6) Uani 1 1 d .
H1 H 0.7278 0.4052 0.8372 0.049 Uiso 1 1 calc GR
C8 C 1.0613(4) 0.2036(4) 0.4077(3) 0.0199(7) Uani 1 1 d .
C12 C 0.8972(4) 0.4193(4) 0.2242(3) 0.0198(7) Uani 1 1 d .
C10 C 1.0677(5) 0.1997(4) 0.1767(4) 0.0235(7) Uani 1 1 d .
C13 C 0.7840(5) 0.5578(4) 0.1748(3) 0.0238(7) Uani 1 1 d .
H13A H 0.6796 0.5619 0.2248 0.036 Uiso 1 1 calc GR
H13B H 0.7587 0.5644 0.0841 0.036 Uiso 1 1 calc GR
H13C H 0.8402 0.6374 0.1832 0.036 Uiso 1 1 calc GR
C11 C 0.9640(5) 0.3314(4) 0.1409(3) 0.0232(7) Uani 1 1 d .
H11 H 0.9372 0.3632 0.0524 0.028 Uiso 1 1 calc R
C5 C 0.5052(4) 0.7487(4) 0.5581(4) 0.0222(7) Uani 1 1 d .
C1 C 0.6028(5) 0.5809(4) 0.7903(4) 0.0243(7) Uani 1 1 d .
C2 C 0.5044(5) 0.6883(4) 0.8413(4) 0.0263(8) Uani 1 1 d .
H2A H 0.4965 0.6767 0.9321 0.032 Uiso 1 1 calc R
C9 C 1.1093(5) 0.1382(4) 0.3039(4) 0.0232(7) Uani 1 1 d .
H9 H 1.1746 0.0458 0.3210 0.028 Uiso 1 1 calc R
C4 C 0.4184(5) 0.8371(4) 0.6329(4) 0.0253(8) Uani 1 1 d .
H4 H 0.3538 0.9232 0.5895 0.030 Uiso 1 1 calc R
C3 C 0.4171(5) 0.8113(4) 0.7673(4) 0.0275(8) Uani 1 1 d .
C6 C 0.4958(5) 0.7867(4) 0.4136(4) 0.0277(8) Uani 1 1 d .
H6A H 0.6040 0.7524 0.3768 0.041 Uiso 1 1 calc GR
H6B H 0.4687 0.8903 0.3859 0.041 Uiso 1 1 calc GR
H6C H 0.4084 0.7420 0.3842 0.041 Uiso 1 1 calc GR
C14 C 1.1365(6) 0.1178(4) 0.0747(4) 0.0332(9) Uani 1 1 d .
H14A H 1.0589 0.1413 0.0022 0.050 Uiso 1 1 calc GR
H14B H 1.1498 0.0154 0.1107 0.050 Uiso 1 1 calc GR
H14C H 1.2457 0.1434 0.0451 0.050 Uiso 1 1 calc GR
C7 C 0.3206(6) 0.9220(5) 0.8356(5) 0.0371(10) Uani 1 1 d .
H7A H 0.2806 0.8748 0.9189 0.056 Uiso 1 1 calc GR
H7B H 0.2245 0.9745 0.7832 0.056 Uiso 1 1 calc GR
H7C H 0.3940 0.9883 0.8490 0.056 Uiso 1 1 calc GR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl1 Cu1 Cu1 115.87(4) . 2_766
Cl1 Cu1 P2 104.33(3) . 2_766
P1 Cu1 Cu1 132.54(4) . 2_766
P1 Cu1 Cl1 103.57(4) . .
P1 Cu1 P2 96.35(3) . 2_766
P2 Cu1 Cu1 50.36(3) 2_766 2_766
P2 Cu1 Cu1 61.74(3) . 2_766
P2 Cu1 Cl1 104.00(3) . .
P2 Cu1 P1 133.39(4) . .
P2 Cu1 P2 112.11(3) . 2_766
C5 P1 Cu1 133.37(13) . .
C5 P1 C1 103.38(18) . .
C1 P1 Cu1 115.06(13) . .
Cu1 P2 Cu1 67.89(3) . 2_766
C8 P2 Cu1 106.20(12) . 2_766
C8 P2 Cu1 117.94(12) . .
C12 P2 Cu1 137.73(13) . .
C12 P2 Cu1 107.31(12) . 2_766
C12 P2 C8 103.90(17) . .
C8 O2 H2 109.5 . .
C1 O1 H1 109.5 . .
O2 C8 P2 121.3(3) . .
O2 C8 C9 116.6(3) . .
C9 C8 P2 122.1(3) . .
C13 C12 P2 118.0(3) . .
C11 C12 P2 121.5(3) . .
C11 C12 C13 120.5(3) . .
C11 C10 C14 119.5(3) . .
C9 C10 C11 122.9(3) . .
C9 C10 C14 117.6(3) . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13B 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C11 C10 125.3(3) . .
C12 C11 H11 117.4 . .
C10 C11 H11 117.4 . .
C4 C5 P1 121.8(3) . .
C4 C5 C6 121.1(3) . .
C6 C5 P1 117.0(3) . .
O1 C1 P1 120.9(3) . .
O1 C1 C2 116.3(3) . .
C2 C1 P1 122.8(3) . .
C1 C2 H2A 118.0 . .
C3 C2 C1 123.9(4) . .
C3 C2 H2A 118.0 . .
C8 C9 H9 117.9 . .
C10 C9 C8 124.2(3) . .
C10 C9 H9 117.9 . .
C5 C4 H4 117.1 . .
C5 C4 C3 125.7(4) . .
C3 C4 H4 117.1 . .
C2 C3 C4 122.4(3) . .
C2 C3 C7 118.2(4) . .
C4 C3 C7 119.4(4) . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6B 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C10 C14 H14A 109.5 . .
C10 C14 H14B 109.5 . .
C10 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C3 C7 H7A 109.5 . .
C3 C7 H7B 109.5 . .
C3 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cu1 2.6976(10) 2_766
Cu1 Cl1 2.3378(9) .
Cu1 P1 2.2534(10) .
Cu1 P2 2.2424(9) .
Cu1 P2 2.5648(10) 2_766
P1 C5 1.736(4) .
P1 C1 1.745(4) .
P2 Cu1 2.5648(10) 2_766
P2 C8 1.752(4) .
P2 C12 1.743(3) .
O2 H2 0.8400 .
O2 C8 1.343(4) .
O1 H1 0.8400 .
O1 C1 1.357(5) .
C8 C9 1.393(5) .
C12 C13 1.506(5) .
C12 C11 1.386(5) .
C10 C11 1.399(5) .
C10 C9 1.392(5) .
C10 C14 1.508(5) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C11 H11 0.9500 .
C5 C4 1.378(5) .
C5 C6 1.506(5) .
C1 C2 1.391(5) .
C2 H2A 0.9500 .
C2 C3 1.388(6) .
C9 H9 0.9500 .
C4 H4 0.9500 .
C4 C3 1.398(6) .
C3 C7 1.513(5) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
