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_7704136
_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         'C63 H82 F3 N5 P2'
_chemical_formula_sum            'C63 H82 F3 N5 P2'
_chemical_formula_weight         1028.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9944(4)
_cell_length_b                   13.1476(2)
_cell_length_c                   19.4279(3)
_cell_measurement_reflns_used    8725
_cell_measurement_temperature    235.01(10)
_cell_measurement_theta_max      72.5810
_cell_measurement_theta_min      3.8240
_cell_volume                     5873.47(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_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      235.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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    -68.00  33.00   1.00   20.00    --  -40.20  57.00  60.00  101
  2  \w   -107.00 -49.00   1.00   20.00    --  -40.20 -57.00 -90.00   58
  3  \w    -75.00  -8.00   1.00   20.00    --  -40.20 125.00-180.00   67
  4  \w    103.00 169.00   1.00   60.00    --  103.61  77.00 -30.00   66
  5  \w    120.00 174.00   1.00   60.00    --  103.61 125.00  30.00   54
  6  \w    108.00 154.00   1.00   60.00    --  103.61  77.00 120.00   46
  7  \w     63.00 125.00   1.00   60.00    --  103.61 -61.00-120.00   62
  8  \w     37.00 136.00   1.00   60.00    --  103.61 -77.00  90.00   99
  9  \w    105.00 170.00   1.00   60.00    --  103.61  77.00-150.00   65
 10  \w    122.00 162.00   1.00   60.00    --  103.61  77.00  90.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0112619000
_diffrn_orient_matrix_UB_12      -0.1127559000
_diffrn_orient_matrix_UB_13      -0.0172556000
_diffrn_orient_matrix_UB_21      0.0600736000
_diffrn_orient_matrix_UB_22      -0.0066338000
_diffrn_orient_matrix_UB_23      -0.0347467000
_diffrn_orient_matrix_UB_31      0.0273982000
_diffrn_orient_matrix_UB_32      -0.0314323000
_diffrn_orient_matrix_UB_33      0.0691291000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22695
_diffrn_reflns_point_group_measured_fraction_full 0.810
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.669
_diffrn_reflns_theta_min         3.362
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 2626 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         9212
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0712P)^2^+0.7032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.550
_reflns_Friedel_fraction_full    0.606
_reflns_Friedel_fraction_max     0.578
_reflns_number_gt                8219
_reflns_number_total             9212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01341b2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7704134--7704141.cif.'
_cod_database_code               7704136
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.919
_diffrn_oxdiff_digest_frames
;
014b48e17a48c00903f5435f244ecfec2a000272ff9
;
_diffrn_oxdiff_digest_hkl
;
0178f81b379d1d5fe99f8f879864eff2126f93
;
_reflns_odcompleteness_completeness 99.95
_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. Uiso/Uaniso restraints and constraints
Uanis(C32) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C37) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(F2) = Uanis(F4) = Uanis(F3A) = Uanis(F3) = Uanis(F0AA) = Uanis(F1A) =
Uanis(F1AA) = Uanis(F2A) = Uanis(F1)
3. Others
 Fixed Sof: F2(0.5) F1(0.5) F3(0.5) F2A(0.3) F3A(0.3) F1A(0.3) F0AA(0.2)
 F1AA(0.2) F4(0.2)
4.a Ternary CH refined with riding coordinates:
 C59(H59), C24(H24), C21(H21), C36(H36), C50(H50), C47(H47), C62(H62), C33(H33)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C39(H39A,H39B), C38(H38A,H38B), C12(H12A,H12B)
4.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C44(H44), C9(H9), C16(H16), C7(H7), C10(H10), C43(H43), C18(H18),
 C6(H6), C28(H28), C56(H56), C17(H17), C29(H29), C55(H55), C54(H54), C30(H30)
4.d Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C60(H60A,H60B,H60C), C20(H20A,H20B,H20C), C63(H63A,
 H63B,H63C), C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C61(H61A,H61B,H61C),
 C37(H37A,H37B,H37C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C22(H22A,H22B,
 H22C), C35(H35A,H35B,H35C)
;
_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 1.126
_oxdiff_exptl_absorpt_empirical_full_min 0.910