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_7037735
_publ_section_title
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 Synthesis and reactions of N-heterocycle functionalised variants of
 heterometallic {Cr7Ni} rings.
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_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_moiety
'C170 H290 Cr14 F16 N2 Ni2 O72 Rh2, 2(C6 H16 N)'
_chemical_formula_sum            'C182 H322 Cr14 F16 N4 Ni2 O72 Rh2'
_chemical_formula_weight         5073.68
_chemical_name_systematic
'[nPr2NH2][Cr7NiF8(O2C5H9)(O2CC5H4N)]2[Re2(O2C2H3)4]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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_update_record
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2015-09-14 deposited with the CCDC.
2015-12-21 downloaded from the CCDC.
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_cell_angle_alpha                90.00
_cell_angle_beta                 111.474(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   56.127(7)
_cell_length_b                   16.2525(19)
_cell_length_c                   31.418(4)
_cell_measurement_temperature    100
_cell_volume                     26670(6)
_computing_molecular_graphics
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
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_computing_publication_material
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            94936
_diffrn_reflns_theta_full        23.84
_diffrn_reflns_theta_max         23.84
_diffrn_reflns_theta_min         2.84
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1540 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.7630.
The \l/2 correction factor is 0.0000.
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_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'clear green'
_exptl_crystal_F_000             10576
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.037
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1334
_refine_ls_number_reflns         15783
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1307P)^2^+174.0757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1943
_refine_ls_wR_factor_ref         0.2173
_reflns_number_gt                11603
_reflns_number_total             15783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04062k2.cif
_cod_data_source_block           GT-136a-09
_cod_depositor_comments
'Adding full bibliography for 7037717--7037737.cif.'
_cod_original_cell_volume        26670(5)
_cod_database_code               7037735
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  H5 of C5, H3 of C3, H4 of C4, {H10K,H10L} of C105, {H1CA,H1CB} of C1C,
  {H1BA,H1BB} of C1B, {H10F,H10G} of C101, {H10D,H10E} of N100, H6 of C6
 At 1.5 times of:
  {H9A,H9B,H9C} of C9, {H25A,H25B,H25C} of C25, {H44A,H44B,H44C} of C44,
  {H24A,H24B,H24C} of C24, {H85A,H85B,H85C} of C85, {H66A,H66B,H66C} of C66,
  {H83A,H83B,H83C} of C83, {H29A,H29B,H29C} of C29, {H14A,H14B,H14C} of C14,
  {H35A,H35B,H35C} of C35, {H70A,H70B,H70C} of C70, {H10H,H10I,H10J} of C106,
  {H50A,H50B,H50C} of C50, {H40A,H40B,H40C} of C40, {H46A,H46B,H46C} of C46,
  {H64A,H64B,H64C} of C64, {H79A,H79B,H79C} of C79, {H56A,H56B,H56C} of C56,
  {H34A,H34B,H34C} of C34, {H45A,H45B,H45C} of C45, {H10A,H10B,H10C} of C10,
  {H65A,H65B,H65C} of C65, {H36A,H36B,H36C} of C36, {H26A,H26B,H26C} of C26,
  {H41A,H41B,H41C} of C41, {H51A,H51B,H51C} of C51, {H16A,H16B,H16C} of C16,
  {H19A,H19B,H19C} of C19, {H15A,H15B,H15C} of C15, {H61A,H61B,H61C} of C61,
  {H80A,H80B,H80C} of C80, {H30A,H30B,H30C} of C30, {H1AA,H1AB,H1AC} of C1A,
  {H74A,H74B,H74C} of C74, {H69A,H69B,H69C} of C69, {H60A,H60B,H60C} of C60,
  {H75A,H75B,H75C} of C75, {H55A,H55B,H55C} of C55, {H49A,H49B,H49C} of C49,
  {H81A,H81B,H81C} of C81, {H76A,H76B,H76C} of C76, {H20A,H20B,H20C} of C20,
  {H71A,H71B,H71C} of C71, {H21A,H21B,H21C} of C21, {H31A,H31B,H31C} of C31,
  {H11A,H11B,H11C} of C11, {H59A,H59B,H59C} of C59, {H54A,H54B,H54C} of C54,
  {H39A,H39B,H39C} of C39
2. Uiso/Uaniso restraints and constraints
C63 ~ C65 ~ C64 ~ C66: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C43 ~ C44 ~ C46 ~ C45: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C23 ~ C24 ~ C25 ~ C26: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C78 ~ C79 ~ C80 ~ C81: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C68 ~ C71 ~ C69 ~ C70: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C58 ~ C61 ~ C59 ~ C60: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C50 ~ C48 ~ C51 ~ C49: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C38 ~ C40 ~ C41 ~ C39: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C29 ~ C28 ~ C30 ~ C31: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C18 ~ C19 ~ C21 ~ C20: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C8 ~ C9 ~ C10 ~ C11: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C75 ~ C76 ~ C73 ~ C74: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C14 ~ C15 ~ C13 ~ C16: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C34 ~ C35 ~ C33 ~ C36: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C54 ~ C55 ~ C53 ~ C56: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Others
 Sof(Ni1A)=Sof(Cr1A)=1-Sof(Cr1A)=1-Sof(Cr1A)
4.a Secondary CH2 refined with riding coordinates:
 N100(H10D,H10E), C101(H10F,H10G), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C105(H10K,
 H10L)
4.b Me refined with riding coordinates:
 C85(H85A,H85B,H85C), C29(H29A,H29B,H29C), C83(H83A,H83B,H83C), C14(H14A,H14B,
 H14C), C35(H35A,H35B,H35C), C24(H24A,H24B,H24C), C44(H44A,H44B,H44C), C25(H25A,
 H25B,H25C), C66(H66A,H66B,H66C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C45(H45A,H45B,H45C), C34(H34A,H34B,H34C), C56(H56A,H56B,H56C), C79(H79A,H79B,
 H79C), C64(H64A,H64B,H64C), C46(H46A,H46B,H46C), C40(H40A,H40B,H40C), C50(H50A,
 H50B,H50C), C65(H65A,H65B,H65C), C36(H36A,H36B,H36C), C26(H26A,H26B,H26C),
 C41(H41A,H41B,H41C), C51(H51A,H51B,H51C), C16(H16A,H16B,H16C), C19(H19A,H19B,
 H19C), C15(H15A,H15B,H15C), C61(H61A,H61B,H61C), C80(H80A,H80B,H80C), C30(H30A,
 H30B,H30C), C39(H39A,H39B,H39C), C54(H54A,H54B,H54C), C59(H59A,H59B,H59C),
 C11(H11A,H11B,H11C), C31(H31A,H31B,H31C), C21(H21A,H21B,H21C), C71(H71A,H71B,
 H71C), C20(H20A,H20B,H20C), C76(H76A,H76B,H76C), C81(H81A,H81B,H81C), C49(H49A,
 H49B,H49C), C55(H55A,H55B,H55C), C75(H75A,H75B,H75C), C60(H60A,H60B,H60C),
 C69(H69A,H69B,H69C), C74(H74A,H74B,H74C), C1A(H1AA,H1AB,H1AC), C106(H10H,H10I,
 H10J), C70(H70A,H70B,H70C)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C3(H3), C4(H4)
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