One-, Two-, and Three-Dimensional Heterospin Complexes Consisting of 4-(N-tert-Butyloxylamino)pyridine (4NOpy), Dicyanamide Ion (DCA), and 3d Metal Ions: Crystal Structures and Magnetic Properties of [M(II)(4NOpy)x(DCA)y(CH3CN)z]n (M = Mn, Co, Ni, Cu, Zn).
Ogawa, Hiraku; Mori, Koya; Murashima, Kensuke; Karasawa, Satoru; Koga, Noboru; Inorganic chemistry 55 (2016) 717–728; doi:10.1021/acs.inorgchem.5b02159

data_4344652
_publ_section_title
;
 One-, Two-, and Three-Dimensional Heterospin Complexes Consisting of
 4-(N-tert-Butyloxylamino)pyridine (4NOpy), Dicyanamide Ion (DCA), and 3d
 Metal Ions: Crystal Structures and Magnetic Properties of
 [M(II)(4NOpy)x(DCA)y(CH3CN)z]n (M = Mn, Co, Ni, Cu, Zn).
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              717
_journal_page_last               728
_journal_paper_doi               10.1021/acs.inorgchem.5b02159
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C15 H16 Cu N9 O'
_chemical_formula_sum            'C15 H16 Cu N9 O'
_chemical_formula_weight         401.90
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                81.625(3)
_cell_angle_beta                 74.034(3)
_cell_angle_gamma                85.718(3)
_cell_formula_units_Z            2
_cell_length_a                   7.204(2)
_cell_length_b                   10.191(3)
_cell_length_c                   12.924(4)
_cell_measurement_temperature    90
_cell_volume                     901.9(5)
_computing_cell_refinement       Unknown
_computing_data_collection       Unknown
_computing_data_reduction        Unknown
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Unknown CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_laue_measured_fraction_full 0.000
_diffrn_reflns_laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4321
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        25.490
_diffrn_reflns_theta_max         25.490
_diffrn_reflns_theta_min         1.653
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             412.00
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.99
_refine_diff_density_min         -0.54
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0689P)^2^+2.7294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                2874
_reflns_number_total             3228
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic5b02159_si_001.cif
_cod_data_source_block           4aCualpha(CCDC1413265)
_cod_original_cell_volume        901.8(4)
_cod_database_code               4344652