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_7037718
_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         'C351 H626 Cr28 Cu2 F32 N12 Ni4 O142.50'
_chemical_formula_sum            'C351 H626 Cr28 Cu2 F32 N12 Ni4 O142.5'
_chemical_formula_weight         9720.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccr4vk8
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-05-20T22:53:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2008-05-30 deposited with the CCDC.
2015-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                83.3020(10)
_cell_angle_beta                 87.7560(10)
_cell_angle_gamma                90.499(3)
_cell_formula_units_Z            2
_cell_length_a                   16.5633(6)
_cell_length_b                   34.1024(10)
_cell_length_c                   48.3098(19)
_cell_measurement_reflns_used    20279
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     27078.3(17)
_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, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.777
_diffrn_measured_fraction_theta_max 0.777
_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      -0.260202E-1
_diffrn_orient_matrix_UB_12      0.256393E-1
_diffrn_orient_matrix_UB_13      0.28865E-2
_diffrn_orient_matrix_UB_21      -0.49527E-1
_diffrn_orient_matrix_UB_22      -0.84313E-2
_diffrn_orient_matrix_UB_23      -0.90489E-2
_diffrn_orient_matrix_UB_31      -0.228331E-1
_diffrn_orient_matrix_UB_32      -0.119759E-1
_diffrn_orient_matrix_UB_33      0.185711E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.153
_diffrn_reflns_av_unetI/netI     0.2618
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            67957
_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        20
_diffrn_reflns_theta_max         20
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.8522
_exptl_absorpt_correction_T_min  0.7897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10172
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.423
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2556
_refine_ls_number_reflns         39277
_refine_ls_number_restraints     29655
_refine_ls_restrained_S_all      1.311
_refine_ls_R_factor_all          0.2643
_refine_ls_R_factor_gt           0.1399
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3019
_refine_ls_wR_factor_ref         0.3331
_reflns_number_gt                13155
_reflns_number_total             39277
_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_formula_sum        'C351 H626 Cr28 Cu2 F32 N12 Ni4 O142.50'
_cod_database_code               7037718