Linked Nickel Metallacrowns from a Phosphonate/2-Pyridyloximate Blend of Ligands: Structure and Magnetic Properties.
Escuer, Albert; Mayans, Júlia; Font-Bardia, Mercè; Inorganic chemistry 55 (2016) 3161–3168; doi:10.1021/acs.inorgchem.6b00103

data_4347381
_publ_section_title
;
 Linked Nickel Metallacrowns from a Phosphonate/2-Pyridyloximate Blend of
 Ligands: Structure and Magnetic Properties.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3161
_journal_page_last               3168
_journal_paper_doi               10.1021/acs.inorgchem.6b00103
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C44 H54 N8 Ni4 O16 P2, 3(C H4 O), 2(H O)'
_chemical_formula_sum            'C47 H68 N8 Ni4 O21 P2'
_chemical_formula_weight         1377.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.751(5)
_cell_angle_beta                 77.748(5)
_cell_angle_gamma                63.279(4)
_cell_formula_units_Z            1
_cell_length_a                   11.8019(15)
_cell_length_b                   12.1788(15)
_cell_length_c                   12.6763(15)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.34
_cell_volume                     1576.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.865
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18057
_diffrn_reflns_point_group_measured_fraction_full 0.865
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.227
_diffrn_reflns_theta_min         2.676
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       prism
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.537
_refine_diff_density_min         -2.420
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4938
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0668P)^2^+7.4029P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3923
_reflns_number_total             4938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00103_si_001.cif
_cod_data_source_block           mo_i06sb28_0ma_aAa
_cod_database_code               4347381