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_7704135
_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         'C56 H78 N4 O P2'
_chemical_formula_sum            'C56 H78 N4 O P2'
_chemical_formula_weight         885.16
_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   difmap
_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                 96.6110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.36670(10)
_cell_length_b                   12.03320(10)
_cell_length_c                   15.31190(10)
_cell_measurement_reflns_used    9454
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.7900
_cell_measurement_theta_min      3.9740
_cell_volume                     2629.48(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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_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    -27.00  21.00   0.50    0.50    --    0.00 -57.00-120.00   96
  2  \w    -86.00   4.00   0.50    0.50    --    0.00 -38.00 -60.00  180
  3  \w    -43.00  14.00   0.50    0.50    --    0.00 -38.00   0.00  114
  4  \w     25.00  50.00   0.50    0.50    --    0.00  38.00   0.00   50
  5  \w    -84.00 -57.00   0.50    0.50    --    0.00 -57.00-120.00   54
  6  \w    120.00 168.00   0.50    2.50    --   95.20  15.00-120.00   96
  7  \w     73.00 105.00   0.50    2.50    --   95.20  15.00-120.00   64
  8  \w      6.00 115.00   0.50    2.50    --   95.20 -45.00 -30.00  218
  9  \w     84.00 185.00   0.50    2.50    --   95.20  30.00 -60.00  202
 10  \w     14.00 119.00   0.50    2.50    --   95.20 -61.00 -30.00  210
 11  \w     74.00 123.00   0.50    2.50    --   95.20  15.00 -90.00   98
 12  \w    105.00 175.00   0.50    2.50    --   95.20  30.00-180.00  140
 13  \w     71.00 100.00   0.50    2.50    --   95.20 -30.00-150.00   58
;
_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      0.0240052000
_diffrn_orient_matrix_UB_12      0.0560974000
_diffrn_orient_matrix_UB_13      0.0902424000
_diffrn_orient_matrix_UB_21      0.1004324000
_diffrn_orient_matrix_UB_22      0.0219421000
_diffrn_orient_matrix_UB_23      -0.0216911000
_diffrn_orient_matrix_UB_31      -0.0314831000
_diffrn_orient_matrix_UB_32      0.1129671000
_diffrn_orient_matrix_UB_33      -0.0405639000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14672
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.121
_diffrn_reflns_theta_min         3.996
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71806
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         5174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0470P)^2^+1.3440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4848
_reflns_number_total             5174
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01341b2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7704134--7704141.cif.'
_cod_database_code               7704135
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.893
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Sof: O1(0.5)
;
_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 1.356
_oxdiff_exptl_absorpt_empirical_full_min 0.734