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_4132574
_publ_section_title
;
 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         'C29 H37 N2 O2 P'
_chemical_formula_sum            'C29 H37 N2 O2 P'
_chemical_formula_weight         476.57
_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
_audit_creation_date             2018-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.170(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8551(14)
_cell_length_b                   10.8440(11)
_cell_length_c                   15.1961(13)
_cell_measurement_reflns_used    5656
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      2.32
_cell_volume                     2571.7(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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0942
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42640
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_min         2.610
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       needle
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0785P)^2^+0.8215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3182
_reflns_number_total             5270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04930_si_002.cif
_cod_data_source_block           2
_cod_database_code               4132574
_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:
 C3(H3), C24(H24), C5(H5), C22(H22)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C26(H26A,H26B,H26C), C8(H8A,H8B,H8C), C17(H17A,H17B,
 H17C), C28(H28A,H28B,H28C), C14(H14A,H14B,H14C), C7(H7A,H7B,H7C), C6(H6A,H6B,
 H6C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              48403
_shelx_hkl_checksum              78964
_olex2_submission_special_instructions 'No special instructions were received'