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_7704138
_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         'C64 H82 N4 P2'
_chemical_formula_sum            'C64 H82 N4 P2'
_chemical_formula_weight         969.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 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                   12.5962(2)
_cell_length_b                   13.0948(2)
_cell_length_c                   34.8018(4)
_cell_measurement_reflns_used    6967
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5420
_cell_measurement_theta_min      3.6000
_cell_volume                     5740.37(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      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 0.973
_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   -111.00 -21.00   1.00    5.00    --  -40.08 -38.00-150.00   90
  2  \w    -36.00   2.00   1.00    5.00    --  -40.08  19.00   0.00   38
  3  \w     50.00  81.00   1.00    5.00    --   40.08 -99.00-180.00   31
  4  \w     37.00 103.00   1.00   20.00    --  105.48 -94.00-120.00   66
  5  \w     81.00 171.00   1.00   20.00    --  105.48  30.00-120.00   90
  6  \w    102.00 170.00   1.00   20.00    --  105.48 125.00-120.00   68
  7  \w     79.00 129.00   1.00   20.00    --  105.48 -45.00  60.00   50
;
_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      -0.0136573000
_diffrn_orient_matrix_UB_12      0.1135610000
_diffrn_orient_matrix_UB_13      0.0105620000
_diffrn_orient_matrix_UB_21      0.0125532000
_diffrn_orient_matrix_UB_22      0.0293509000
_diffrn_orient_matrix_UB_23      -0.0426219000
_diffrn_orient_matrix_UB_31      -0.1208423000
_diffrn_orient_matrix_UB_32      -0.0097064000
_diffrn_orient_matrix_UB_33      -0.0055906000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            14864
_diffrn_reflns_point_group_measured_fraction_full 0.878
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.393
_diffrn_reflns_theta_min         3.606
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.122
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 3093 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0483P)^2^+1.3742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.556
_reflns_Friedel_fraction_full    0.729
_reflns_Friedel_fraction_max     0.672
_reflns_number_gt                9110
_reflns_number_total             9701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01341b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7704134--7704141.cif.'
_cod_database_code               7704138
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.804
_reflns_odcompleteness_completeness 99.72
_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 Everything fixed:
 H2
2.b Ternary CH refined with riding coordinates:
 C37(H37), C25(H25), C63(H63), C22(H22), C51(H51), C48(H48), C34(H34), C60(H60)
2.c Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C39(H39A,H39B), C13(H13A,H13B), C14(H14A,H14B)
2.d Aromatic/amide H refined with riding coordinates:
 C45(H45), C17(H17), C11(H11), C29(H29), C19(H19), C18(H18), C43(H43),
 C12(H12), C44(H44), C57(H57), C10(H10), C31(H31), C9(H9), C30(H30), C8(H8),
 C56(H56), C55(H55)
2.e Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C26(H26A,H26B,H26C), C47(H47A,H47B,H47C), C23(H23A,H23B,
 H23C), C33(H33A,H33B,H33C), C64(H64A,H64B,H64C), C35(H35A,H35B,H35C), C24(H24A,
 H24B,H24C), C49(H49A,H49B,H49C), C62(H62A,H62B,H62C), C61(H61A,H61B,H61C),
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C38(H38A,H38B,H38C), C59(H59A,H59B,
 H59C), C21(H21A,H21B,H21C)
;
_olex2_date_sample_data_collection 2019-03-08
_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 1.412
_oxdiff_exptl_absorpt_empirical_full_min 0.769