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_4320441
_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            'C45 H56 Cl N4 O5 P'
_chemical_formula_weight         799.39
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.323(4)
_cell_length_b                   12.523(2)
_cell_length_c                   16.406(4)
_cell_measurement_temperature    298
_cell_measurement_theta_max      60
_cell_measurement_theta_min      56
_cell_volume                     4380.9(15)
_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 1.0003
_diffrn_measured_fraction_theta_max 1.0003
_diffrn_measurement_device       'Mac Science MXC3'
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.009
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            4148
_diffrn_reflns_theta_full        64.21
_diffrn_reflns_theta_max         64.21
_exptl_absorpt_coefficient_mu    14.04
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1704.00
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     505
_refine_ls_number_reflns         3260
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.0130
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00766|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                3260
_reflns_number_total             3793
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ic010595e_06.cif
_cod_data_source_block           OEPPPhOnPr+ClO4-(6f-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_cell_volume        4381(2)
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C45 H56 Cl N4 O5 P '
_cod_database_code               4320441