A Room-Temperature-Stable Phosphanorcaradiene.
Liu, Liu Leo; Zhou, Jiliang; Andrews, Ryan; Stephan, Douglas W.; Journal of the American Chemical Society 140 (2018) 7466–7470; doi:10.1021/jacs.8b04930

data_4132575
_publ_section_title
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 A Room-Temperature-Stable Phosphanorcaradiene.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7466
_journal_page_last               7470
_journal_paper_doi               10.1021/jacs.8b04930
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C43 H45 N2 O4 P'
_chemical_formula_sum            'C43 H45 N2 O4 P'
_chemical_formula_weight         684.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                99.452(4)
_cell_angle_beta                 103.114(3)
_cell_angle_gamma                95.605(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8219(11)
_cell_length_b                   13.2831(16)
_cell_length_c                   14.8369(18)
_cell_measurement_reflns_used    5829
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      2.32
_cell_volume                     1841.2(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39808
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.448
_diffrn_reflns_theta_min         2.747
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0576 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.9631.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.6481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4940
_reflns_number_total             7529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04930_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
;

2020-09-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         342.39
_cod_original_formula_moiety         '0.5(C43 H45 N2 O4 P)'
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C21.50 H22.50 N O2 P0.50'
_cod_database_code               4132575
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C32(H32), C23(H23), C19(H19), C25(H25), C10(H10), C11(H11),
 C12(H12), C16(H16), C13(H13), C18(H18), C17(H17)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C42(H42A,H42B,H42C), C5(H5A,H5B,H5C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C),
  C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              56066
_shelx_hkl_checksum              63342
_olex2_submission_special_instructions 'No special instructions were received'