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_4347383
_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_absolute_configuration rm
_chemical_formula_moiety
'C102 H105 N24 Ni8 O21 P3, Cl3 Cs O12, 2(Cl O4), C H4 O'
_chemical_formula_sum            'C103 H109 Cl5 Cs N24 Ni8 O42 P3'
_chemical_formula_weight         3227.89
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0420(13)
_cell_length_b                   23.0420(13)
_cell_length_c                   23.0420(13)
_cell_measurement_reflns_used    9745
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.50
_cell_volume                     12233.8(12)
_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 0.844
_diffrn_measured_fraction_theta_max 0.998
_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  0.0719
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.844
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            116705
_diffrn_reflns_point_group_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         23.565
_diffrn_reflns_theta_min         2.500
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    1.741
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       prism
_exptl_crystal_F_000             6560
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.204
_refine_diff_density_max         0.990
_refine_diff_density_min         -4.511
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details
;
 Flack x determined using 2475 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.031(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         6073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1290P)^2^+109.0957P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2016
_refine_ls_wR_factor_ref         0.2068
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.838
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5676
_reflns_number_total             6073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00103_si_001.cif
_cod_data_source_block           mo_I06SB31_0ma_a
_cod_original_cell_volume        12234(2)
_cod_database_code               4347383