Synthesis, magnetism, 1H NMR and redox activity of dicopper(II) complexes having a discrete {Cu2(μ-phenoxide)2}2+ unit supported by a non-macrocyclic ligand environment. Crystal structure of [Cu2(L)2(OClO3)2] [HL = 4-methyl-2,6-bis(pyrazol-1-ylmethyl)phenol] †
Gupta, Rajeev; Mukherjee, Sumitra; Mukherjee, Rabindranath; Journal of the Chemical Society, Dalton Transactions  (1999) 4025–; doi:10.1039/a907250k

data_7027794
_publ_contact_author
;
     ? name        Professor R. Mukherjee 
     ? institute   Indian Institute of Technology 
     ? department  Chemistry  
     ? address     I.I.T. Kanpur 208 016
     ? city        Kanpur 
     ? country     India   
;
_publ_section_title
;
 Synthesis, magnetism, 1H NMR and redox activity of dicopper(II) complexes
 having a discrete {Cu2(\m-phenoxide)2}2+ unit supported by a
 non-macrocyclic ligand environment. Crystal structure of
 [Cu2(L)2(OClO3)2]
 [HL&#x2005;=&#x2005;4-methyl-2,6-bis(pyrazol-1-ylmethyl)phenol]&#x200A;&#x2020;
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4025
_journal_paper_doi               10.1039/a907250k
_journal_year                    1999
_chemical_compound_source        'Synthesized in the laboratory   '
_chemical_formula_analytical     'Cu2 Cl2 O10 N8 C30 H30'
_chemical_formula_moiety         'Cu2 C30 H30 N8 O2 2+, Cl2 O8 2-'
_chemical_formula_structural     ' (Cu2 C30 H30 N8 O2) (ClO4)2   '
_chemical_formula_sum            'C30 H30 Cl2 Cu2 N8 O10'
_chemical_formula_weight         860
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   ' position calculated '
_atom_sites_solution_primary     'Cu, Cl '
_atom_sites_solution_secondary   ' rest non hydrogen atoms '
_audit_creation_date             99-00-08
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                96.55(2)
_cell_angle_beta                 110.168(7)
_cell_angle_gamma                115.77(3)
_cell_formula_units_Z            1
_cell_length_a                   10.0850(8)
_cell_length_b                   10.249(5)
_cell_length_c                   10.472(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      21.9
_cell_measurement_theta_min      11.8
_cell_volume                     869.2(5)
_computing_data_collection       'CAD4mach-PC version   '
_computing_data_reduction        xtal_DIFDAT_ADDREFF_SORTRF_ABSORB
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'theta-2 theta    '
_diffrn_radiation_detector       'proportional counter       '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed xray_tube  '
_diffrn_radiation_type           'Mo K-alpha     '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .017
_diffrn_reflns_av_sigmaI/netI    .019
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3246
_diffrn_reflns_reduction_process No_monochr_Lp_applied
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0.303
_diffrn_standards_interval_time  'every hour  '
_diffrn_standards_number         three
_exptl_absorpt_coefficient_mu    1.45
_exptl_absorpt_correction_T_max  0.5685
_exptl_absorpt_correction_T_min  0.5637
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       ' Rectangular plate    '
_exptl_crystal_F_000             437.9
_exptl_crystal_preparation
'ethyl acetate diffusion to acetonitrile solution   '
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.33
_refine_diff_density_min         -.834
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_expression No
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.236
_refine_ls_goodness_of_fit_obs   1.253
_refine_ls_hydrogen_treatment    No
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2528
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .052
_refine_ls_R_factor_obs          .043
_refine_ls_shift/esd_max         '0.1940 x 10-3 '
_refine_ls_shift/esd_mean        '0.7790 x 10-5'
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_all         .056
_refine_ls_wR_factor_obs         .051
_reflns_d_resolution_high        .84
_reflns_d_resolution_low         9.339
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              10
_reflns_limit_k_min              -12
_reflns_limit_l_max              11
_reflns_limit_l_min              -12
_reflns_number_observed          2528
_reflns_number_total             3056
_reflns_observed_criterion       refl_observed_if_Inet_>_.000_sigma(Inet)
_cod_data_source_file            907250ksup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        869.3(5)
_cod_original_sg_symbol_Hall     -P_1
_cod_original_sg_symbol_H-M      P1~
_cod_original_formula_sum        '  Cu2 Cl2 O10 N8 C30 H30    '
_cod_database_code               7027794