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_7704139
_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         'C57 H80 N4 O P2'
_chemical_formula_sum            'C57 H80 N4 O P2'
_chemical_formula_weight         899.19
_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                 94.2270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.42330(10)
_cell_length_b                   33.6427(3)
_cell_length_c                   12.62960(10)
_cell_measurement_reflns_used    19703
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.7940
_cell_measurement_theta_min      2.6150
_cell_volume                     5264.23(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)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.975
_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    -89.00 -40.00   0.50    0.50    --    0.00 -38.00   0.00   98
  2  \w    -82.00 -16.00   0.50    0.50    --    0.00 -57.00  90.00  132
  3  \w    -89.00 -15.00   0.50    0.50    --    0.00 -38.00-180.00  148
  4  \w     72.00 171.00   0.50    2.50    --   95.20  61.00-150.00  198
  5  \w     62.00 127.00   0.50    2.50    --   95.20 -82.00  90.00  130
  6  \w    150.00 176.00   0.50    2.50    --   95.20  45.00 -30.00   52
  7  \w     79.00 182.00   0.50    2.50    --   95.20  30.00 -60.00  206
  8  \w     79.00 185.00   0.50    2.50    --   95.20  30.00 -90.00  212
  9  \w     16.00  81.00   0.50    2.50    --   95.20 -77.00  60.00  130
 10  \w     43.00 119.00   0.50    2.50    --   95.20 -61.00  60.00  152
 11  \w     12.00  85.00   0.50    2.50    --   95.20 -30.00 120.00  146
 12  \w     26.00  51.00   0.50    2.50    --   95.20 -30.00  60.00   50
;
_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      -0.0366253000
_diffrn_orient_matrix_UB_12      0.0316647000
_diffrn_orient_matrix_UB_13      0.0778036000
_diffrn_orient_matrix_UB_21      0.0065906000
_diffrn_orient_matrix_UB_22      -0.0310122000
_diffrn_orient_matrix_UB_23      0.0899552000
_diffrn_orient_matrix_UB_31      0.1186589000
_diffrn_orient_matrix_UB_32      0.0115039000
_diffrn_orient_matrix_UB_33      0.0285338000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33317
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.203
_diffrn_reflns_theta_min         2.627
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93752
_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    1.135
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0455P)^2^+2.2913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9717
_reflns_number_total             10457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01341b2.cif
_cod_data_source_block           8b
_cod_depositor_comments
'Adding full bibliography for 7704134--7704141.cif.'
_cod_database_code               7704139
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.849
_reflns_odcompleteness_completeness 99.93
_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. Others
 Fixed Sof: P2(0.18) P2A(0.82) H2A(0.5) H2(0.5)
3.a Ternary CH refined with riding coordinates:
 C15(H15), C27(H27), C56(H56), C44(H44), C53(H53), C30(H30), C18(H18), C41(H41)
3.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C6(H6A,H6B), C7(H7A,H7B), C32(H32A,H32B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C22(H22), C48(H48), C10(H10), C36(H36), C11(H11), C24(H24),
 C50(H50), C49(H49), C23(H23), C37(H37), C38(H38)
3.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C28(H28A,H28B,H28C), C55(H55A,H55B,
 H55C), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C52(H52A,
 H52B,H52C), C54(H54A,H54B,H54C), C57(H57A,H57B,H57C), C31(H31A,H31B,H31C),
 C29(H29A,H29B,H29C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C)
;
_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 1.355
_oxdiff_exptl_absorpt_empirical_full_min 0.887