Reactivity in polynuclear transition metal chemistry as a means to obtain high-spin molecules: substitution of µ4-OH‒ by η1,µ4-N3‒ increases nine times the ground-state S value of a nonanuclear nickel(ii) cage
Papaefstathiou, Giannis S.; Escuer, Albert; Vicente, Ramon; Font-Bardia, Merce; Solans, Xavier; Perlepes, Spyros P.; Chemical Communications  (2001) 2414–; doi:10.1039/b106472j

data_7114974
_publ_section_title
;
 Reactivity in polynuclear transition metal chemistry as a means to obtain
 high-spin molecules: substitution of &#x00B5;4-OH-- by \h1,&#x00B5;4-N3--
 increases nine times the ground-state S value of a nonanuclear nickel(ii)
 cage
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2414
_journal_paper_doi               10.1039/b106472j
_journal_year                    2001
_chemical_formula_moiety
'C60 H56 N14 NI9 O24  4 (C3 H7 N O)  4.5(H2O)'
_chemical_formula_sum            'C72 H93 N18 Ni9 O32.5'
_chemical_formula_weight         2258.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.841(8)
_cell_length_b                   17.841(8)
_cell_length_c                   14.008(3)
_cell_measurement_reflns_used    23354
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.89
_cell_measurement_theta_min      2.71
_cell_volume                     4459(3)
_computing_cell_refinement       MARXDS
_computing_data_collection       MARXDS
_computing_data_reduction        MARSCALE
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.819
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measurement_device_type  'mar2400 - image plate detector'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24451
_diffrn_reflns_theta_full        28.89
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    1.948
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
phi-scan, North, Phillips and Mathews, 1968, Acta Cryst, A24, 351-359
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.074
_refine_ls_extinction_expression Fc
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.215
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                3417
_reflns_number_total             5241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106472j.txt
_cod_data_source_block           complex_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P4/n
_cod_original_formula_sum        'C72 H93 N18 Ni9 O32.50'
_cod_database_code               7114974