Room temperature stable <i>E</i>,<i>Z</i>-diphosphenes: their isomerization, coordination, and cycloaddition chemistry.
Lin, Jieli; Liu, Shihua; Zhang, Jie; Grützmacher, Hansjörg; Su, Cheng-Yong; Li, Zhongshu; Chemical science 14 (2023) 10944–10952; doi:10.1039/d3sc04506d

data_1569856
_publ_section_title
;
 Room temperature stable <i>E</i>,<i>Z</i>-diphosphenes: their
 isomerization, coordination, and cycloaddition chemistry.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              10944
_journal_page_last               10952
_journal_paper_doi               10.1039/d3sc04506d
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C62 H88 N4 P2'
_chemical_formula_sum            'C62 H88 N4 P2'
_chemical_formula_weight         951.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-06-20 deposited with the CCDC.	2023-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.295(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9163(17)
_cell_length_b                   14.6645(10)
_cell_length_c                   31.890(3)
_cell_measurement_reflns_used    4524
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.4780
_cell_measurement_theta_min      2.7000
_cell_volume                     5943.1(11)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.860
_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     51.00  81.00   0.15   50.00    --    0.00  19.00   0.00  200
  2  \w    -89.00 -32.00   0.15   50.00    --    0.00 -43.00  55.61  380
  3  \w    -18.00   9.00   0.15   50.00    --    0.00 -43.00  55.61  180
  4  \w      3.00  29.10   0.15   50.00    --    0.00  38.00 -90.00  174
  5  \w     33.00  59.10   0.15   50.00    --    0.00  38.00 -90.00  174
  6  \w      0.00  26.10   0.15   50.00    --    0.00  38.00   0.00  174
  7  \w    -89.00 -47.00   0.15   50.00    --    0.00 -77.00 -60.00  280
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0279342000
_diffrn_orient_matrix_UB_12      -0.0418243000
_diffrn_orient_matrix_UB_13      0.0013759000
_diffrn_orient_matrix_UB_21      -0.0277415000
_diffrn_orient_matrix_UB_22      -0.0153701000
_diffrn_orient_matrix_UB_23      0.0158412000
_diffrn_orient_matrix_UB_31      -0.0393429000
_diffrn_orient_matrix_UB_32      -0.0188974000
_diffrn_orient_matrix_UB_33      -0.0160837000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            50772
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.862
_diffrn_reflns_theta_min         2.392
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93213
_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    1.063
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         14724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0885P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10055
_reflns_number_total             14724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04506d2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 1569855--1569860.cif.'
_cod_original_cell_volume        5943.0(11)
_cod_database_code               1569856
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23), C32(H32), C35(H35), C46(H46), C49(H49), C58(H58), C61(H61)
1.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C37(H37A,H37B),
 C38(H38A,H38B)
1.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28), C29(H29),
 C41(H41), C42(H42), C43(H43), C53(H53), C54(H54), C55(H55)
1.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C45(H45A,H45B,H45C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C57(H57A,H57B,
 H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C)
;
_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 1.909
_oxdiff_exptl_absorpt_empirical_full_min 0.850