One-dimensional Co(II)/Ni(II) complexes of 2-hydroxyisophthalate: Structures and magnetic properties
Wang, Kai; Zou, Hua-Hong; Chen, Zi-Lu; Zhang, Zhong; Sun, Wei-Yin; Liang, Fu-Pei; Journal of Solid State Chemistry 226 (2015) 36–41; doi:10.1016/j.jssc.2015.01.029

data_1561939
_publ_section_title
;
 One-dimensional Co(II)/Ni(II) complexes of 2-hydroxyisophthalate:
 Structures and magnetic properties
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              36
_journal_page_last               41
_journal_paper_doi               10.1016/j.jssc.2015.01.029
_journal_volume                  226
_journal_year                    2015
_chemical_formula_moiety         '2(C18 H16 Co N2 O6)'
_chemical_formula_sum            'C36 H32 Co2 N4 O12'
_chemical_formula_weight         830.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 106.359(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8431(5)
_cell_length_b                   9.1292(2)
_cell_length_c                   20.7267(5)
_cell_measurement_temperature    296.15
_cell_volume                     3602.67(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30509
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.00033(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         6329
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.9463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                5542
_reflns_number_total             6329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2015-226-36.cif
_cod_data_source_block           422
_cod_original_cell_volume        3602.67(15)
_cod_database_code               1561939
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O6-H1 = O6-H2
 0.85 with sigma of 0.01
 H1-H2
 1.4 with sigma of 0.02
 O12-H17 = O12-H18
 0.85 with sigma of 0.01
 H17-H18
 1.4 with sigma of 0.02
3.a Riding coordinates:
 O2(H17,H2,H1,H18)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H5), C5(H12), C4(H6), C23(H22), C31(H27), C27(H23), C14(H4), C13(H10),
 C17(H15), C36(H32), C11(H11), C10(H8), C9(H7), C15(H13), C18(H16), C32(H28),
 C34(H30), C35(H31), C12(H9), C30(H26), C33(H29), C16(H14), C28(H24), C29(H25),
 C21(H20), C22(H21)
;