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_4347384
_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_sum            'C102 H97.5 N12 Na2 Ni8 O33 P3'
_chemical_formula_weight         2627.98
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   18.6908(8)
_cell_length_b                   18.6908(8)
_cell_length_c                   22.3049(9)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.52
_cell_volume                     6748.2(5)
_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-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_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  0.0504
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            50846
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.382
_diffrn_reflns_theta_min         2.218
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       prism
_exptl_crystal_F_000             2697
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 1835 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.001(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4742
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0654P)^2^+3.5000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4374
_reflns_number_total             4742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00103_si_001.cif
_cod_data_source_block           mo_i06sb21_0m_a_a_sq_d
_cod_depositor_comments
;

2024-02-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C204 H195 N24 Na4 Ni16 O66 P6'
_cod_original_formula_weight         5255.97
_cod_original_formula_units_Z            1
_cod_original_cell_volume        6748.2(6)
_cod_database_code               4347384
_shelxl_version_number           2012-9
_shelx_res_checksum              95776
_shelx_hkl_checksum              32838