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_7037723
_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            'C87 H155 Cr7 F8 N2 Ni O32'
_chemical_formula_weight         2315.84
_chemical_name_systematic        '[nPr2NH2][Cr7NiF8(O2C5H9)15(O2CC5H4N)]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-14 deposited with the CCDC.
2015-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.127(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.141(3)
_cell_length_b                   17.059(2)
_cell_length_c                   30.727(4)
_cell_measurement_reflns_used    8276
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      2.35
_cell_volume                     12660(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 and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6933
_diffrn_reflns_av_R_equivalents  0.1128
_diffrn_reflns_av_sigmaI/netI    0.0994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            61732
_diffrn_reflns_theta_full        21.49
_diffrn_reflns_theta_max         21.49
_diffrn_reflns_theta_min         3.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_correction_T_min  0.9612
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4860
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O/MeCN'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.321
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         14465
_refine_ls_number_restraints     1311
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1416
_refine_ls_R_factor_gt           0.0986
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1595P)^2^+40.9014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2640
_refine_ls_wR_factor_ref         0.3017
_reflns_number_gt                9093
_reflns_number_total             14465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04062k2.cif
_cod_data_source_block           p21c
_cod_depositor_comments
'Adding full bibliography for 7037717--7037737.cif.'
_cod_original_cell_volume        12659(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7037723