"ortho-Wurster's Crowns": Synthesis and Properties of a Novel Phenylenediamine-Based Redox-Active Macrocyclic Ligand
John W. Sibert; Philip B. Forshee; Inorganic Chemistry 41 (2002) 5928–5930; doi:10.1021/ic0259235

data_4318879
_publ_section_title
;
 "ortho-Wurster's Crowns": Synthesis and Properties of a Novel
 Phenylenediamine-Based Redox-Active Macrocyclic Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5928
_journal_page_last               5930
_journal_paper_doi               10.1021/ic0259235
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C5.08 H8.63 F1.52 K0.25 N0.51 O1.27 P0.25'
_chemical_formula_weight         143.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            63
_cell_length_a                   18.912(4)
_cell_length_b                   18.447(4)
_cell_length_c                   30.856(6)
_cell_measurement_temperature    293(2)
_cell_volume                     10765(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            26161
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.330
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_F_000             4736
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.212
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         6928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.212
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_obs          0.0633
_refine_ls_shift/esd_max         0.257
_refine_ls_shift/esd_mean        0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2200
_refine_ls_wR_factor_obs         0.1947
_reflns_number_observed          4222
_reflns_number_total             6930
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0259235-4_s2.cif
_cod_data_source_block           earb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10764.7(37)
_cod_database_code               4318879