New class of phosphine oxide donor-based supramolecular coordination complexes from an in situ phosphine oxidation reaction or phosphine oxide ligands.
Shankar, Bhaskaran; Elumalai, Palani; Shanmugam, Ramasamy; Singh, Virender; Masram, Dhanraj T.; Sathiyendiran, Malaichamy; Inorganic chemistry 52 (2013) 10217–10219; doi:10.1021/ic401257w

data_4338350
_publ_section_title
;
 New class of phosphine oxide donor-based supramolecular coordination
 complexes from an in situ phosphine oxidation reaction or phosphine oxide
 ligands.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10217
_journal_page_last               10219
_journal_paper_doi               10.1021/ic401257w
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C74 H56 O22 P4 Re4, C9 H12'
_chemical_formula_sum            'C83 H68 O22 P4 Re4'
_chemical_formula_weight         2286.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 105.803(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   19.166(5)
_cell_length_b                   16.682(5)
_cell_length_c                   27.879(5)
_cell_measurement_reflns_used    22652
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.00
_cell_volume                     8577(4)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2011)'
_computing_data_collection       'CrysAlis RED (Oxford, 2011)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2011)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            74744
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    5.771
_exptl_absorpt_correction_T_max  0.3770
_exptl_absorpt_correction_T_min  0.2518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4408
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.21
_refine_diff_density_max         8.277
_refine_diff_density_min         -4.909
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         15068
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+207.3380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                12080
_reflns_number_total             15068
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic401257w_si_002.cif
_cod_data_source_block           ep1-136-2
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4338350