Formation of dinuclear macrocyclic and mononuclear acyclic complexes of a new trinucleating hexaaza triphenolic Schiff base macrocycle: structure and NLO properties
Korupoju, Srinivas R.; Mangayarkarasi, Nagarathinam; Ameerunisha, Sardar; Valente, Edward J.; Zacharias, Panthappally S.; Journal of the Chemical Society, Dalton Transactions  (2000) 2845–; doi:10.1039/b002700f

data_7009683
_publ_section_title
;
 Formation of dinuclear macrocyclic and mononuclear acyclic complexes
 of a new trinucleating hexaaza triphenolic Schiff base macrocycle:
 structure and NLO properties
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2845
_journal_paper_doi               10.1039/b002700f
_journal_year                    2000
_chemical_compound_source        'Hodgson (MSU) 1996'
_chemical_formula_sum            'C34 H40 Cl Cu2 N5 O8'
_chemical_formula_weight         809.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 109.56(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.042(11)
_cell_length_b                   19.769(9)
_cell_length_c                   12.477(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     3729(4)
_computing_cell_refinement       'P3 (Siemens Analytical Xray Inc.)'
_computing_data_collection       'P3 (Siemens Analytical Xray Inc.)'
_computing_data_reduction        'XDISK (Siemens Analytical Xray Inc.)'
_computing_molecular_graphics    'XP (Siemens Analytical Xray Inc.)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'scintillation counter, PH analysis'
_diffrn_measurement_method       'omega scans, 2.0 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1821
_diffrn_reflns_av_sigmaI/netI    0.1734
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6341
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%
' mean -10.3 (min -39.4; max +3.9), solvent loss'
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  1.5h
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  na
_exptl_absorpt_correction_T_min  na
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'brown (transmission), black (reflectance)'
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    na
_exptl_crystal_description       'flat, prismatic'
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.221
_refine_ls_goodness_of_fit_obs   1.742
_refine_ls_hydrogen_treatment    'calculated, fixed, riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         5225
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.246
_refine_ls_restrained_S_obs      1.689
_refine_ls_R_factor_all          0.2134
_refine_ls_R_factor_obs          0.0835
_refine_ls_shift/esd_max         0.020
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2157
_refine_ls_wR_factor_obs         0.1809
_reflns_number_observed          2226
_reflns_number_total             5227
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002700f.txt
_cod_data_source_block           '[Cu2L3(OAc)]ClO4CH3CN'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'na' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0720P)^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^)+(0.0720P)^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        3728.5(36)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009683