Structural and spectroscopic characterization of copper(II) complexes of a new bisamide functionalized imidazole tripod and evidence for the formation of a mononuclear end-on Cu-OOH species.
Cheruzel, Lionel E.; Cecil, Matthew R.; Edison, Sara E.; Mashuta, Mark S.; Baldwin, Michael J.; Buchanan, Robert M.; Inorganic chemistry 45 (2006) 3191–3202; doi:10.1021/ic051280s

data_4350115
_publ_section_title
;
 Structural and spectroscopic characterization of copper(II) complexes of
 a new bisamide functionalized imidazole tripod and evidence for the
 formation of a mononuclear end-on Cu-OOH species.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3191
_journal_page_last               3202
_journal_paper_doi               10.1021/ic051280s
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C25 H40 N9 Cu O3, Cl O4'
_chemical_formula_sum            'C25 H40 Cl Cu N9 O7'
_chemical_formula_weight         677.66
_chemical_name_common            '[Cu(L2)OH]ClO4'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 93.766(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.653(10)
_cell_length_b                   10.260(5)
_cell_length_c                   31.194(15)
_cell_measurement_reflns_used    12328
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      1.89
_cell_volume                     6915(6)
_computing_cell_refinement       'SAINT 6.36 (Bruker, 2001)'
_computing_data_collection       'SMART 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT 6.36 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-99 (Sheldrick, 1999)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       \w-scans
_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  0.1149
_diffrn_reflns_av_sigmaI/netI    0.1787
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            49657
_diffrn_reflns_theta_full        25.18
_diffrn_reflns_theta_max         25.18
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Sheldrick, G. M.; SADABS (1996).

;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2818
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         12328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1944
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1806
_reflns_number_gt                4542
_reflns_number_total             12328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051280ssi20050729_115254.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_moiety     'C50 H80 N18 Cu2 O6, Cl2 O8'
_cod_original_formula_sum        'C50 H80 Cl2 Cu2 N18 O14'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1355.32
_cod_database_code               4350115