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_7704137
_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         'C62 H82 N4 O P2'
_chemical_formula_sum            'C62 H82 N4 O P2'
_chemical_formula_weight         961.25
_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                 99.4350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.71500(10)
_cell_length_b                   22.9346(2)
_cell_length_c                   21.8186(2)
_cell_measurement_reflns_used    18347
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.8390
_cell_measurement_theta_min      2.8120
_cell_volume                     6276.53(10)
_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 0.972
_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    -17.00  18.00   0.50    0.50    --    0.00  57.00 -30.00   70
  2  \w    -41.00  16.00   0.50    0.50    --    0.00 -38.00  90.00  114
  3  \w    -20.00  18.00   0.50    0.50    --    0.00 -19.00 150.00   76
  4  \w     51.00  89.00   0.50    0.50    --    0.00  57.00 -30.00   76
  5  \w     61.00  87.00   0.50    0.50    --    0.00  38.00  60.00   52
  6  \w     47.00 127.00   0.50    1.14    --   95.20 -82.00 150.00  160
  7  \w     80.00 106.00   0.50    1.14    --   95.20 -82.00 120.00   52
  8  \w      9.00  86.00   0.50    1.14    --   95.20 -30.00  60.00  154
  9  \w     10.00  70.00   0.50    1.14    --   95.20 -61.00  90.00  120
 10  \w     15.00 118.00   0.50    1.14    --   95.20 -61.00 150.00  206
 11  \w     79.00 181.00   0.50    1.14    --   95.20  15.00-180.00  204
 12  \w     46.00  99.00   0.50    1.14    --   95.20 -45.00 -60.00  106
 13  \w    119.00 173.00   0.50    1.14    --   95.20  45.00  30.00  108
 14  \w      8.00  33.00   0.50    1.14    --   95.20 -77.00-120.00   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      0.1200444000
_diffrn_orient_matrix_UB_12      -0.0119191000
_diffrn_orient_matrix_UB_13      0.0033586000
_diffrn_orient_matrix_UB_21      -0.0150541000
_diffrn_orient_matrix_UB_22      -0.0023782000
_diffrn_orient_matrix_UB_23      -0.0714957000
_diffrn_orient_matrix_UB_31      0.0210686000
_diffrn_orient_matrix_UB_32      0.0660428000
_diffrn_orient_matrix_UB_33      -0.0019882000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36570
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.142
_diffrn_reflns_theta_min         2.816
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76597
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_description       needle
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         12416
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0653P)^2^+2.3401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10936
_reflns_number_total             12416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01341b2.cif
_cod_data_source_block           8c
_cod_depositor_comments
'Adding full bibliography for 7704134--7704141.cif.'
_cod_original_cell_volume        6276.52(10)
_cod_database_code               7704137
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.771
_reflns_odcompleteness_completeness 99.92
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C62-C61
 1.5 with sigma of 0.0001
 C63-C61
 1.5 with sigma of 0.0001
3. Others
 Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Fixed Sof: H61(0.7) H61A(0.3) C62(0.7) H62A(0.7) H62B(0.7) H62C(0.7) C63(0.3)
 H63A(0.3) H63B(0.3) H63C(0.3)
4.a Ternary CH refined with riding coordinates:
 C20(H20), C35(H35), C23(H23), C32(H32), C46(H46), C58(H58), C49(H49),
 C61(H61), C61(H61A)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C11(H11C,H11D), C37(H37A,H37B), C38(H38A,H38B), C12(H12A,
 H12B), C12A(H12C,H12D)
4.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C15(H15), C10(H10), C6(H6), C9(H9), C55(H55), C41(H41),
 C7(H7), C42(H42), C8(H8), C43(H43), C54(H54), C53(H53), C27(H27), C29(H29),
 C28(H28)
4.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C45(H45A,H45B,H45C), C19(H19A,H19B,H19C), C31(H31A,H31B,
 H31C), C22(H22A,H22B,H22C), C57(H57A,H57B,H57C), C24(H24A,H24B,H24C), C48(H48A,
 H48B,H48C), C59(H59A,H59B,H59C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C),
 C33(H33A,H33B,H33C), C50(H50A,H50B,H50C), C47(H47A,H47B,H47C), C60(H60A,H60B,
 H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C)
;
_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 1.388
_oxdiff_exptl_absorpt_empirical_full_min 0.649