Low-Valent Chemistry: An Alternative Approach to Phosphorus-Containing Oligomers.
Kosnik, Stephanie C.; Farrar, Gregory J.; Norton, Erin L.; Cooper, Benjamin F. T.; Ellis, Bobby D.; Macdonald, Charles L. B.; Inorganic chemistry  (2014) 141201074418004–; doi:10.1021/ic502229w

data_4341816
_publ_section_title
;
 Low-Valent Chemistry: An Alternative Approach to Phosphorus-Containing
 Oligomers.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141201074418004
_journal_paper_doi               10.1021/ic502229w
_journal_year                    2014
_chemical_formula_moiety         'C58 H46 P6, 0.81(C4 H10 O)'
_chemical_formula_sum            'C61.26 H54.17 O0.81 P6'
_chemical_formula_weight         989.25
_chemical_name_systematic
;
 ?
;
_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_method           SHELXL-2012
_cell_angle_alpha                86.0290(10)
_cell_angle_beta                 74.7350(10)
_cell_angle_gamma                83.9100(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6149(11)
_cell_length_b                   13.2909(12)
_cell_length_c                   17.6210(16)
_cell_measurement_reflns_used    3083
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.91
_cell_volume                     2831.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_unetI/netI     0.1347
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30110
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.437
_diffrn_reflns_theta_min         1.199
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2012'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             1037
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Squeeze was used to remove a set of chemically unreasonable peaks
located/disordered about the inversion center.  The R values prior
to the Squeeze treatment were:
_refine_ls_R_factor_all           0.1979
_refine_ls_R_factor_gt            0.1459
_refine_ls_wR_factor_ref          0.3914
_refine_ls_wR_factor_gt           0.3546
;
_refine_diff_density_max         1.250
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         11528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.1055
_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/[\s^2^(Fo^2^)+(0.0707P)^2^+10.8574P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2217
_refine_ls_wR_factor_ref         0.2427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7476
_reflns_number_total             11528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502229w_si_007.cif
_cod_data_source_block           shelx
_cod_database_code               4341816
_shelxl_version_number           2012-9
_shelx_res_checksum              59736
_shelx_hkl_checksum              95049