Synthesis, Structure, Electrochemistry, and Spectroelectrochemistry of Hypervalent Phosphorus(V) Octaethylporphyrins and Theoretical Analysis of the Nature of the PO Bond in P(OEP)(CH2CH3)(O)
Kin-ya Akiba; Ryo Nadano; Wataru Satoh; Yohsuke Yamamoto; Shigeru Nagase; Zhongping Ou; Xiaoyu Tan; Karl M. Kadish; Inorganic Chemistry 40 (2001) 5553–5567; doi:10.1021/ic010595e

data_4320442
_publ_section_title
;
 Synthesis, Structure, Electrochemistry, and Spectroelectrochemistry of
 Hypervalent Phosphorus(V) Octaethylporphyrins and Theoretical Analysis of
 the Nature of the PO Bond in P(OEP)(CH2CH3)(O)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5553
_journal_page_last               5567
_journal_paper_doi               10.1021/ic010595e
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C40 H55 Cl N5 O4 P'
_chemical_formula_weight         736.33
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                87.84(5)
_cell_angle_beta                 85.58(5)
_cell_angle_gamma                63.32(5)
_cell_formula_units_Z            2
_cell_length_a                   9.845(6)
_cell_length_b                   10.946(8)
_cell_length_c                   21.67(1)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298
_cell_measurement_theta_max      30
_cell_measurement_theta_min      19
_cell_volume                     2080(2)
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 1.0041
_diffrn_measured_fraction_theta_max 1.0041
_diffrn_measurement_device       'Mac Science MXC3'
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.013
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5675
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_exptl_absorpt_coefficient_mu    1.36
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             788.00
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.14
_refine_diff_density_min         -1.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.957
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     411
_refine_ls_number_reflns         2526
_refine_ls_R_factor_gt           0.1307
_refine_ls_shift/su_max          0.0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.01000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2012
_reflns_number_gt                2526
_reflns_number_total             5445
_reflns_threshold_expression     F^2^>4.0\s(F^2^)
_cod_data_source_file            ic010595e_07.cif
_cod_data_source_block           OEPPEt(NEt2)+ClO4-(7a-ClO4)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C40 H55 Cl N5 O4 P '
_cod_database_code               4320442