Facile addition of E-H bonds to a dicarbondiphosphide.
Zhang, Xu; Chen, Xiaodan; Zhai, Haojiang; Liu, Shihua; Hu, Chenyang; Liu, Liu Leo; Wang, Shuhai; Li, Zhongshu; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6384–6390; doi:10.1039/d0dt01341b

data_7704141
_publ_section_title
;
 Facile addition of E-H bonds to a dicarbondiphosphide.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6384
_journal_page_last               6390
_journal_paper_doi               10.1039/d0dt01341b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '4(C63 H82 N6 P2)'
_chemical_formula_sum            'C256 H334 N26 P8'
_chemical_formula_weight         4023.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-20 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.906(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.2082(9)
_cell_length_b                   21.2732(9)
_cell_length_c                   22.2484(8)
_cell_measurement_reflns_used    11567
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.0370
_cell_measurement_theta_min      3.3090
_cell_volume                     12338.4(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.969
_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     31.00  88.00   0.50   50.00    --    0.00  38.00  60.00  114
  2  \w     19.00  88.00   0.50   50.00    --    0.00  38.00 150.00  138
  3  \w    -15.00  11.00   0.50   50.00    --    0.00  38.00 150.00   52
  4  \w      3.00  87.00   0.50   50.00    --    0.00  19.00 -60.00  168
  5  \w    -30.00  -5.00   0.50   50.00    --    0.00 -57.00-180.00   50
  6  \w     81.00 107.00   0.50  100.00    --   95.20 -30.00  90.00   52
  7  \w     79.00 159.00   0.50  100.00    --   95.20  45.00-180.00  160
  8  \w      6.00 125.00   0.50  100.00    --   95.20 -77.00 -30.00  238
  9  \w     14.00  54.00   0.50  100.00    --   95.20 -61.00  30.00   80
 10  \w     29.00 114.00   0.50  100.00    --   95.20 -45.00  60.00  170
 11  \w     77.00 163.00   0.50  100.00    --   95.20  61.00-120.00  172
 12  \w     24.00  99.00   0.50  100.00    --   95.20 -61.00 -30.00  150
 13  \w    103.00 169.00   0.50  100.00    --   95.20  45.00 150.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0323350000
_diffrn_orient_matrix_UB_12      -0.0414543000
_diffrn_orient_matrix_UB_13      0.0383524000
_diffrn_orient_matrix_UB_21      -0.0494182000
_diffrn_orient_matrix_UB_22      0.0289652000
_diffrn_orient_matrix_UB_23      -0.0319283000
_diffrn_orient_matrix_UB_31      -0.0017362000
_diffrn_orient_matrix_UB_32      -0.0518376000
_diffrn_orient_matrix_UB_33      -0.0485215000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0982
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73158
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.446
_diffrn_reflns_theta_min         2.681
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       block
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         24449
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0806P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13212
_reflns_number_total             24449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01341b2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7704134--7704141.cif.'
_cod_database_code               7704141
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.911
_reflns_odcompleteness_completeness 99.89
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C37, C36
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C100) \\sim Ueq, Uanis(C101) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(H99A)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(H97C)=Sof(C100)=Sof(H10J)=
 Sof(H10K)=Sof(H10L)=1-FVAR(1)
 Sof(H99)=Sof(C101)=Sof(H10G)=Sof(H10H)=Sof(H10I)=Sof(C98)=Sof(H98A)=Sof(H98B)=
 Sof(H98C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C124(H124), C21(H21), C127(H127), C99(H99), C99(H99A), C112(H112), C89(H89),
 C103(H103), C33(H33), C24(H24), C62(H62), C36(H36), C86(H86), C48(H48),
 C59(H59), C45(H45), C115(H115)
5.b Secondary CH2 refined with riding coordinates:
 C68(H68A,H68B), C12(H12M,H12N), C69(H69A,H69B), C77(H77A,H77B), C13(H13A,
 H13B), C50(H50A,H50B), C51(H51A,H51B), C78(H78A,H78B)
5.c Aromatic/amide H refined with riding coordinates:
 N11(H11), N5(H5), C6(H6), C71(H71), C119(H119), C121(H121), C74(H74),
 C93(H93), C7(H7), C75(H75), C72(H72), C16(H16), C95(H95), C120(H120), C9(H9),
 C10(H10), C17(H17), C94(H94), C18(H18), C81(H81), C83(H83), C40(H40), C29(H29),
  C30(H30), C41(H41), C82(H82), C56(H56), C42(H42), C109(H109), C54(H54),
 C28(H28), C108(H108), C55(H55), C107(H107)
5.d Idealised Me refined as rotating group:
 C123(H12A,H12B,H12C), C22(H22A,H22B,H22C), C88(H88A,H88B,H88C), C90(H90A,H90B,
 H90C), C104(H10A,H10B,H10C), C102(H10D,H10E,H10F), C20(H20A,H20B,H20C),
 C85(H85A,H85B,H85C), C113(H11A,H11B,H11C), C126(H12D,H12E,H12F), C58(H58A,H58B,
 H58C), C61(H61A,H61B,H61C), C111(H11D,H11E,H11F), C125(H12G,H12H,H12I),
 C37(H37A,H37B,H37C), C87(H87A,H87B,H87C), C32(H32A,H32B,H32C), C35(H35A,H35B,
 H35C), C63(H63A,H63B,H63C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C34(H34A,
 H34B,H34C), C128(H12J,H12K,H12L), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C),
 C114(H11G,H11H,H11I), C116(H11J,H11K,H11L), C46(H46A,H46B,H46C), C60(H60A,H60B,
 H60C), C44(H44A,H44B,H44C), C101(H10G,H10H,H10I), C98(H98A,H98B,H98C),
 C97(H97A,H97B,H97C), C100(H10J,H10K,H10L)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.107
_oxdiff_exptl_absorpt_empirical_full_min 0.721