Synthesis and reactions of N-heterocycle functionalised variants of heterometallic {Cr7Ni} rings.
Whitehead, George F. S.; Ferrando-Soria, Jesús; Carthy, Laura; Pritchard, Robin G.; Teat, Simon J.; Timco, Grigore A.; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1638–1647; doi:10.1039/c5dt04062k

data_7037728
_publ_section_title
;
 Synthesis and reactions of N-heterocycle functionalised variants of
 heterometallic {Cr7Ni} rings.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1638
_journal_page_last               1647
_journal_paper_doi               10.1039/c5dt04062k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C184 H312 Cr14 Cu F28 N4 Ni2 O68'
_chemical_formula_weight         5109.32
_chemical_name_systematic
'[nPr2NH2][Cr7NiF8(O2C5H9)(O2CC5H4N)]2[Cu(hfac)2]'
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-08-08T09:55:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-09-14 deposited with the CCDC.
2015-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                99.150(3)
_cell_angle_beta                 98.927(3)
_cell_angle_gamma                112.035(2)
_cell_formula_units_Z            1
_cell_length_a                   16.4384(6)
_cell_length_b                   16.7162(6)
_cell_length_c                   26.8666(12)
_cell_measurement_temperature    90(2)
_cell_volume                     6567.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52091
_diffrn_reflns_theta_full        28.2
_diffrn_reflns_theta_max         28.2
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6112
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2661.0
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O/MeCN'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.0005(3)
_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   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1358
_refine_ls_number_reflns         24212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1029P)^2^+5.5432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2098
_reflns_number_gt                16431
_reflns_number_total             24212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04062k2.cif
_cod_data_source_block           gt413b_08
_cod_depositor_comments
'Adding full bibliography for 7037717--7037737.cif.'
_cod_original_cell_volume        6567.5(4)
_cod_original_formula_sum        'C184 H312 Cr14 Cu F28 N4 Ni2 O68 '
_cod_database_code               7037728