Crystal structures of bis- and hexakis[(6,6'-dihydroxybipyridine)copper(II)] nitrate coordination complexes
Gerlach, Deidra L.; Nieto, Ismael; Herbst-Gervasoni, Corey J.; Ferrence, Gregory M.; Zeller, Matthias; Papish, Elizabeth T.; Acta Crystallographica Section E 71 (2015) 1447–1453; doi:10.1107/S205698901502037X

data_2241290
_publ_section_title
;
 Crystal structures of bis- and
 hexakis[(6,6'-dihydroxybipyridine)copper(II)] nitrate coordination
 complexes
;
_journal_coeditor_code           LH5780
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1447
_journal_page_last               1453
_journal_paper_doi               10.1107/S205698901502037X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[Cu6 (C10 H6 N2 O2)2 (C H4 O)2 (O H)4 (N O3)4 (C10 H8 N2 O2)4]'
_chemical_formula_moiety         'C62 H56 Cu6 N16 O30'
_chemical_formula_sum            'C62 H56 Cu6 N16 O30'
_chemical_formula_weight         1886.53
_chemical_name_common
'[Cu3(C10H8N2O2)2(C10H6N2O2)(CH3OH)(OH)2(NO3)2]2'
_chemical_name_systematic
Bis(\m~3~-bipyridine-2,2'-diolato-\k^3^<i>O</i>:<i>N</i>,<i>N</i>':<i>O</i>')tetrakis(6,6'-dihydroxybipyridine-\k^2^<i>N</i>,<i>N</i>')tetrakis(\m-hydroxido-\k^2^<i>O</i>:<i>O</i>')bis(methanol-\k<i>O</i>)tetrakis(\m-nitrato-\k^2^<i>O</i>:<i>O</i>')hexacopper(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                64.591(4)
_cell_angle_beta                 75.659(5)
_cell_angle_gamma                82.262(5)
_cell_formula_units_Z            1
_cell_length_a                   10.2135(7)
_cell_length_b                   13.3707(8)
_cell_length_c                   14.0565(10)
_cell_measurement_reflns_used    1117
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      3.01
_cell_volume                     1679.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2012 (Sheldrick, 2015),
<i>SHELXLE</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20719
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.002
_diffrn_reflns_theta_min         1.641
_exptl_absorpt_coefficient_mu    1.972
_exptl_absorpt_correction_T_max  0.746347
_exptl_absorpt_correction_T_min  0.621924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2009)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_description       prism
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.900
_refine_diff_density_min         -1.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         10920
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0680P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                7847
_reflns_number_total             10920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5780sup1.cif
_cod_data_source_block           II
_cod_database_code               2241290
_cod_database_fobs_code          2241290
_shelx_hkl_checksum              80464
_shelx_res_checksum              37722
_shelxl_version_number           .002012