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_7037737
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C194 H346 Cr14 Cu2 F16 N4 Ni2 O72'
_chemical_formula_sum            'C192 H344 Cr14 Cu2 F16 N6 Ni2 O72'
_chemical_formula_weight         5165.23
_chemical_name_common            'Compound X'
_chemical_name_systematic
'[nPr2NH2][Cr7NiF8(O2C5H9)(O2CC4H3N2)]2[Cu2(O2C5H9)4]'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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             2013-08-08T14:26:32-00:00
_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                90
_cell_angle_beta                 103.9900(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   60.7106(12)
_cell_length_b                   16.7468(4)
_cell_length_c                   30.4987(9)
_cell_measurement_reflns_used    15645
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.967
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     30088.5(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.153074E-1
_diffrn_orient_matrix_UB_12      -0.254369E-1
_diffrn_orient_matrix_UB_13      -0.97688E-2
_diffrn_orient_matrix_UB_21      0.15056E-2
_diffrn_orient_matrix_UB_22      -0.207967E-1
_diffrn_orient_matrix_UB_23      0.313221E-1
_diffrn_orient_matrix_UB_31      -0.71812E-2
_diffrn_orient_matrix_UB_32      0.498607E-1
_diffrn_orient_matrix_UB_33      0.80807E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1218
_diffrn_reflns_av_unetI/netI     0.1524
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21941
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        18.85
_diffrn_reflns_theta_max         18.85
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.8875
_exptl_absorpt_correction_T_min  0.8099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10832.0
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.453
_refine_diff_density_min         -0.6
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         11718
_refine_ls_number_restraints     1278
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.2378
_refine_ls_R_factor_gt           0.1339
_refine_ls_shift/su_max          0.11
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3447
_refine_ls_wR_factor_ref         0.4096
_reflns_number_gt                5227
_reflns_number_total             11718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04062k2.cif
_cod_data_source_block           rob
_cod_depositor_comments
'Adding full bibliography for 7037717--7037737.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C192 H344 Cr14 Cu2 F16 N6 Ni2 O72 '
_cod_database_code               7037737