First entry into nonmetal-centred porphycenes: synthesis of a phosphorus(v) complex of octaethylporphycene.
Abe, Masaaki; Mukotaka, Hiroto; Fujioka, Taro; Okawara, Toru; Umegaki, Kei; Ono, Toshikazu; Hisaeda, Yoshio; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2487–2491; doi:10.1039/c7dt04471b

data_7701899
_publ_section_title
;
 First entry into nonmetal-centred porphycenes: synthesis of a
 phosphorus(v) complex of octaethylporphycene.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2487
_journal_page_last               2491
_journal_paper_doi               10.1039/c7dt04471b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C38 H50 N4 O2 P, F6 P'
_chemical_formula_sum            'C38 H50 F6 N4 O2 P2'
_chemical_formula_weight         770.76
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.4690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0495(9)
_cell_length_b                   8.8372(6)
_cell_length_c                   29.5665(18)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.25
_cell_volume                     3824.1(4)
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            45576
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         1.407
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8115
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+2.5932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6909
_reflns_number_total             8115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04471b2.cif
_cod_data_source_block           mkt2_0m
_cod_database_code               7701899
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.919
_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. Uiso/Uaniso restraints and constraints
Uanis(F6A) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F2A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C29A) = Uanis(C12)
3. Others
 Sof(F2A)=Sof(F3A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(C29A)=Sof(H29c)=Sof(H29d)=Sof(C30A)=Sof(H30d)=Sof(H30e)=Sof(H30f)=1-FVAR(2)
 Sof(C29)=Sof(H29a)=Sof(H29b)=Sof(C30)=Sof(H30a)=Sof(H30b)=Sof(H30c)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b), C23(H23a,H23b), C25(H25a,H25b), C27(H27a,H27b), C29(H29a,
 H29b), C29A(H29c,H29d), C31(H31a,H31b), C33(H33a,H33b), C35(H35a,H35b)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C15(H15), C20(H20)
4.c Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C24(H24a,H24b,H24c), C26(H26a,H26b,H26c), C28(H28a,H28b,
 H28c), C30(H30a,H30b,H30c), C30A(H30d,H30e,H30f), C32(H32a,H32b,H32c),
 C34(H34a,H34b,H34c), C36(H36a,H36b,H36c), C37(H37a,H37b,H37c), C38(H38a,H38b,
 H38c)
;
_shelx_res_checksum              19127
_olex2_submission_special_instructions 'No special instructions were received'