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_7704134
_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         '2(C56 H77 N4 P2), 2(C3 H N2), C6 H5 F'
_chemical_formula_sum            'C124 H161 F N12 P4'
_chemical_formula_weight         1962.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                 93.9800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9039(3)
_cell_length_b                   16.3725(2)
_cell_length_c                   38.5734(5)
_cell_measurement_reflns_used    26592
_cell_measurement_temperature    149.97(10)
_cell_measurement_theta_max      73.7410
_cell_measurement_theta_min      3.4820
_cell_volume                     12539.9(3)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.960
_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     12.00  38.00   0.50    4.94    --    0.00  38.00-180.00   52
  2  \w     -8.00  50.00   0.50    4.94    --    0.00  38.00 -90.00  116
  3  \w    -44.00  16.00   0.50    4.94    --    0.00 -38.00  90.00  120
  4  \w    -37.00  -3.00   0.50    4.94    --    0.00 -57.00-150.00   68
  5  \w    -88.00 -16.00   0.50    4.94    --    0.00 -57.00  60.00  144
  6  \w     73.00 175.00   0.50   19.77    --   95.20  15.00 150.00  204
  7  \w      6.00 115.00   0.50   19.77    --   95.20 -61.00-180.00  218
  8  \w    157.00 182.00   0.50   19.77    --   95.20  15.00  90.00   50
  9  \w     88.00 114.00   0.50   19.77    --   95.20 -77.00  90.00   52
 10  \w     24.00  63.00   0.50   19.77    --   95.20 -77.00  90.00   78
 11  \w     80.00 154.00   0.50   19.77    --   95.20  15.00  90.00  148
 12  \w      6.00 101.00   0.50   19.77    --   95.20 -45.00-180.00  190
 13  \w      6.00  90.50   0.50   19.77    --   95.20 -30.00 -60.00  169
;
_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      0.0675993000
_diffrn_orient_matrix_UB_12      -0.0456651000
_diffrn_orient_matrix_UB_13      -0.0004297000
_diffrn_orient_matrix_UB_21      -0.0136317000
_diffrn_orient_matrix_UB_22      -0.0161837000
_diffrn_orient_matrix_UB_23      -0.0391963000
_diffrn_orient_matrix_UB_31      0.0355519000
_diffrn_orient_matrix_UB_32      0.0806822000
_diffrn_orient_matrix_UB_33      -0.0081171000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            72764
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.334
_diffrn_reflns_theta_min         2.574
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77372
_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 orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_description       block
_exptl_crystal_F_000             4232
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         24562
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0753
_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^)+(0.0681P)^2^+20.5340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20686
_reflns_number_total             24562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01341b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7704134--7704141.cif.'
_cod_database_code               7704134
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.912
_reflns_odcompleteness_completeness 99.67
_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. Restrained distances
 F1-C136
 1.5 with sigma of 0.002
 H3-C62
 2.55 with sigma of 0.001
3. Rigid bond restraints
 C89A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Uiso/Uaniso restraints and constraints
Uanis(C104) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C89) \\sim Ueq: with sigma of 0.004 and
sigma for terminal atoms of 0.008
Uanis(C45) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(C104) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C89A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C18A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Sof(H46A)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(1)
 Sof(H46)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(1)
 Sof(H17A)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(2)
 Sof(H17)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(2)
 Sof(H88A)=Sof(C89A)=Sof(H89D)=Sof(H89E)=Sof(H89F)=1-FVAR(3)
 Sof(H88)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C58(H58), C114(H114), C105(H105), C55(H55), C32(H32), C117(H117), C29(H29),
 C46(H46), C46(H46A), C79(H79), C76(H76), C102(H102), C91(H91), C20(H20),
 C17(H17), C17(H17A), C43(H43), C88(H88), C88(H88A)
6.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C35(H35A,H35B), C93(H93A,H93B), C9(H9A,H9B), C8(H8A,H8B),
 C94(H94A,H94B), C67(H67A,H67B), C68(H68A,H68B)
6.c Aromatic/amide H refined with riding coordinates:
 C52(H52), C51(H51), C50(H50), C71(H71), C111(H111), C26(H26), C99(H99),
 C72(H72), C109(H109), C110(H110), C25(H25), C73(H73), C24(H24), C40(H40),
 C97(H97), C83(H83), C39(H39), C98(H98), C38(H38), C85(H85), C84(H84), C65(H65),
  C12(H12), C14(H14), C6(H6), C13(H13), C135(H135), C134(H134), C133(H133),
 C132(H132), C131(H131)
6.d Fitted hexagon refined as free rotating group:
 C136(C135,C134,C133,C132,C131)
6.e Idealised Me refined as rotating group:
 C113(H11A,H11B,H11C), C115(H11D,H11E,H11F), C31(H31A,H31B,H31C), C75(H75A,
 H75B,H75C), C59(H59A,H59B,H59C), C101(H10A,H10B,H10C), C44(H44A,H44B,H44C),
 C57(H57A,H57B,H57C), C78(H78A,H78B,H78C), C56(H56A,H56B,H56C), C28(H28A,H28B,
 H28C), C87(H87A,H87B,H87C), C106(H10D,H10E,H10F), C118(H11G,H11H,H11I),
 C80(H80A,H80B,H80C), C47(H47A,H47B,H47C), C103(H10G,H10H,H10I), C116(H11J,H11K,
 H11L), C30(H30A,H30B,H30C), C90(H90A,H90B,H90C), C77(H77A,H77B,H77C), C19(H19A,
 H19B,H19C), C54(H54A,H54B,H54C), C33(H33A,H33B,H33C), C92(H92A,H92B,H92C),
 C21(H21A,H21B,H21C), C42(H42A,H42B,H42C), C104(H10J,H10K,H10L), C89(H89A,H89B,
 H89C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C45(H45A,H45B,H45C),
 C45A(H45D,H45E,H45F), C18A(H18D,H18E,H18F), C89A(H89D,H89E,H89F)
;
_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 1.571
_oxdiff_exptl_absorpt_empirical_full_min 0.697