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_1550499
_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         '2(C92 H76 Cu4 O4 P8), 3(C H2 Cl2)'
_chemical_formula_sum            'C187 H158 Cl6 Cu8 O8 P16'
_chemical_formula_weight         3749.66
_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             2018-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                87.081(3)
_cell_angle_beta                 75.816(3)
_cell_angle_gamma                63.403(4)
_cell_formula_units_Z            1
_cell_length_a                   14.7461(6)
_cell_length_b                   15.0636(7)
_cell_length_c                   22.9640(7)
_cell_measurement_reflns_used    37364
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.63
_cell_volume                     4412.0(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.1760
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37269
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.634
_exptl_absorpt_coefficient_mu    1.237
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             1918
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         15005
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.847
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0488P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7359
_reflns_number_total             15005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05281f2.cif
_cod_data_source_block           fp090115
_cod_original_cell_volume        4412.0(3)
_cod_database_code               1550499
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1A-Cl4
 1.74 with sigma of 0.001
 C1A-Cl3
 1.74 with sigma of 0.001
3. Others
 Fixed Sof: Cl3(0.5) Cl4(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5)
4.a Free rotating group:
 Cl3(Cl4,C1A)
4.b Secondary CH2 refined with riding coordinates:
 C93(H93A,H93B), C1A(H1AA,H1AB)
4.c Aromatic/amide H refined with riding coordinates:
 C64(H64), C28(H28), C13(H13), C35(H35), C16(H16), C11(H11), C9(H9), C17(H17),
 C6(H6), C67(H67), C68(H68), C18(H18), C34(H34), C8(H8), C44(H44), C32(H32),
 C7(H7), C40(H40), C86(H86), C2(H2), C22(H22), C12(H12), C1(H1), C70(H70),
 C29(H29), C65(H65), C23(H23), C72(H72), C49(H49), C52(H52), C19(H19), C66(H66),
  C14(H14), C78(H78), C58(H58), C82(H82), C30(H30), C71(H71), C77(H77),
 C48(H48), C4(H4), C47(H47), C31(H31), C46(H46), C50(H50), C41(H41), C55(H55),
 C59(H59), C74(H74), C62(H62), C92(H92), C38(H38), C36(H36), C26(H26), C53(H53),
  C37(H37), C76(H76), C56(H56), C90(H90), C89(H89), C91(H91), C88(H88),
 C80(H80), C61(H61), C3(H3), C73(H73), C42(H42), C25(H25), C85(H85), C43(H43),
 C24(H24), C54(H54), C79(H79), C83(H83), C60(H60), C84(H84)
;
_olex2_submission_special_instructions 'No special instructions were received'