Metastable phosphorus neutral monoradical: a key intermediate in the bicyclic cage formation.
Chen, Xiaodan; Hinz, Alexander; Harmer, Jeffrey R.; Li, Zhongshu; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2549–2553; doi:10.1039/c8dt04842h

data_7048641
_publ_section_title
;
 Metastable phosphorus neutral monoradical: a key intermediate in the
 bicyclic cage formation.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2549
_journal_page_last               2553
_journal_paper_doi               10.1039/c8dt04842h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C46 H70 N2 O2 P2, 2(C6 D6)'
_chemical_formula_sum            'C58 H70 D12 N2 O2 P2'
_chemical_formula_weight         913.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-13 deposited with the CCDC.
2019-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 131.533(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.4871(13)
_cell_length_b                   10.2236(2)
_cell_length_c                   22.3739(10)
_cell_measurement_reflns_used    8659
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      74.1930
_cell_measurement_theta_min      4.7500
_cell_volume                     5049.1(6)
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_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   -109.00 -17.00   1.00   20.00    --  -41.14 -38.00 -30.00   92
  2  \w    -66.00  24.00   1.00   20.00    --  -41.14  38.00 150.00   90
  3  \w    -74.00  26.00   1.00   20.00    --  -41.14  77.00-120.00  100
  4  \w     54.00 121.00   1.00   40.00    --  107.98 -30.00  90.00   67
  5  \w    144.00 172.00   1.00   40.00    --  107.98  30.00 -60.00   28
  6  \w     30.00 109.00   1.00   40.00    --  107.98 -95.00 150.00   79
  7  \w     93.00 141.00   1.00   40.00    --  107.98  30.00 -60.00   48
  8  \w     32.00 134.00   1.00   40.00    --  107.98 -30.00 -90.00  102
  9  \w     35.00 120.00   1.00   40.00    --  107.98-125.00  90.00   85
 10  \w    101.00 172.00   1.00   40.00    --  107.98 125.00-150.00   71
 11  \w     80.00 123.00   1.00   40.00    --  107.98  30.00 -90.00   43
 12  \w    151.00 177.00   1.00   40.00    --  107.98  30.00 -90.00   26
 13  \w     32.00 134.00   1.00   40.00    --  107.98 -77.00-120.00  102
;
_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      0.0180624000
_diffrn_orient_matrix_UB_12      0.1453763000
_diffrn_orient_matrix_UB_13      0.0187856000
_diffrn_orient_matrix_UB_21      -0.0673271000
_diffrn_orient_matrix_UB_22      0.0393578000
_diffrn_orient_matrix_UB_23      -0.0616770000
_diffrn_orient_matrix_UB_31      -0.0035777000
_diffrn_orient_matrix_UB_32      -0.0045945000
_diffrn_orient_matrix_UB_33      0.0656094000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13877
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.123
_diffrn_reflns_theta_min         3.984
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67641
_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 orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0600P)^2^+3.3840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4560
_reflns_number_total             5019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04842h2.cif
_cod_data_source_block           exp_1466
_cod_depositor_comments
'Adding full bibliography for 7048639--7048641.cif.'
_cod_original_cell_volume        5049.1(5)
_cod_database_code               7048641
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B), C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C15(H15), C24(D24), C29(D29), C28(D28), C25(D25),
 C27(D27), C26(D26)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C23(H23A,H23B,H23C),
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C)
;
_olex2_date_sample_data_collection 2017-05-26
_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 2.574
_oxdiff_exptl_absorpt_empirical_full_min 0.782