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_4344650
_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         'C26 H32 N12 Ni O2'
_chemical_formula_sum            'C26 H32 N12 Ni O2'
_chemical_formula_weight         603.32
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.892(5)
_cell_length_b                   11.012(4)
_cell_length_c                   23.526(9)
_cell_measurement_temperature    90
_cell_volume                     3081(2)
_computing_cell_refinement       Unknown
_computing_data_collection       Unknown
_computing_data_reduction        Unknown
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0381
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16035
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1264.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         1.690
_refine_diff_density_min         -0.240
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1429 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.355(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4866
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0618P)^2^+1.3499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                4303
_reflns_number_total             4868
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic5b02159_si_001.cif
_cod_data_source_block           3Nialpha(CCDC1413264)
_cod_database_code               4344650