Synthesis and Crystal Structure Determination of Some Asymmetrical and Symmetrical CR-Type Macrocyclic Schiff Base Complexes, with a Single Pendant Coordinating 2-Aminoethyl Arm
Hassan Keypour; Sadegh Salehzadeh; Robin G. Pritchard; R. V. Parish; Inorganic Chemistry 39 (2000) 5787–5790; doi:10.1021/ic000511m

data_4321656
_publ_contact_author
;
        Prof. H. Keypour
        Department of Chemistry
        University of Bu Ali Sina
        Hamadan
        Iran
;
_publ_contact_author_email       keypour@basu.ac.ir
_publ_contact_author_fax         '0098 81 8272404'
_publ_contact_author_phone       '0098 81 8223283'
_publ_section_title
;
 Synthesis and Crystal Structure Determination of Some Asymmetrical and
 Symmetrical CR-Type Macrocyclic Schiff Base Complexes, with a Single
 Pendant Coordinating 2-Aminoethyl Arm
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5787
_journal_page_last               5790
_journal_paper_doi               10.1021/ic000511m
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C18 H29 Cu F12 N5 P2'
_chemical_formula_weight         668.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.73(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.366(3)
_cell_length_b                   15.549(3)
_cell_length_c                   20.283(2)
_cell_measurement_temperature    295(2)
_cell_volume                     2607.9(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1527
_diffrn_reflns_av_sigmaI/netI    0.1243
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4757
_diffrn_reflns_theta_full        65.10
_diffrn_reflns_theta_max         65.10
_diffrn_reflns_theta_min         4.41
_exptl_absorpt_coefficient_mu    3.330
_exptl_absorpt_correction_T_max  0.7318
_exptl_absorpt_correction_T_min  0.4349
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         4431
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1800
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.2140
_reflns_number_gt                1884
_reflns_number_total             4431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000511m_1.cif
_cod_data_source_block           ra
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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        2607.8(11)
_cod_database_code               4321656