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_4320445
_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            'C39 H52 Cl2 F6 N4 P2'
_chemical_formula_weight         823.71
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_cell_angle_alpha                90
_cell_angle_beta                 100.94(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.584(2)
_cell_length_b                   18.202(3)
_cell_length_c                   9.600(2)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    298
_cell_measurement_theta_max      32
_cell_measurement_theta_min      24
_cell_volume                     1987.4(6)
_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 0.7836
_diffrn_measured_fraction_theta_max 0.7836
_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       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3918
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_exptl_absorpt_coefficient_mu    2.57
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             864.00
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.434
_refine_ls_number_parameters     268
_refine_ls_number_reflns         1825
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.0091
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00774|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                1825
_reflns_number_total             3642
_reflns_threshold_expression     F^2^>4.0\s(F^2^)
_cod_data_source_file            ic010595e_10.cif
_cod_data_source_block           OEPPMe2+PF6-(11a-PF6)
_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        1987.2(5)
_cod_original_formula_sum        'C39 H52 Cl2 F6 N4 P2 '
_cod_database_code               4320445