Single and double nitroxide labeled bis(terpyridine)-copper(ii): influence of orientation selectivity and multispin effects on PELDOR and RIDME.
Meyer, Andreas; Abdullin, Dinar; Schnakenburg, Gregor; Schiemann, Olav; Physical chemistry chemical physics : PCCP 18 (2016) 9262–9271; doi:10.1039/c5cp07621h

data_7224460
_publ_section_title
;
 Single and double nitroxide labeled bis(terpyridine)-copper(ii):
 influence of orientation selectivity and multispin effects on PELDOR and
 RIDME.
;
_journal_issue                   13
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              9262
_journal_page_last               9271
_journal_paper_doi               10.1039/c5cp07621h
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety
'C88 H70 Cu N8 O6, 2(F6 P), 4.5(C3 H6 O), C6 H12'
_chemical_formula_sum            'C107.5 H109 Cu F12 N8 O10.5 P2'
_chemical_formula_weight         2034.50
_chemical_name_systematic        AM30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-08 deposited with the CCDC.
2016-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                71.678(3)
_cell_angle_beta                 67.478(3)
_cell_angle_gamma                86.691(3)
_cell_formula_units_Z            4
_cell_length_a                   20.1608(8)
_cell_length_b                   22.3481(8)
_cell_length_c                   25.7380(10)
_cell_measurement_reflns_used    12136
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      2.60
_cell_volume                     10142.9(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.2945
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62874
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         2.598
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.9395
_exptl_absorpt_correction_T_min  0.6176
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE XRed'
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       needle
_exptl_crystal_F_000             4244
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.717
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2573
_refine_ls_number_reflns         36067
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      0.728
_refine_ls_R_factor_all          0.1895
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0276P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11323
_reflns_number_total             36067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cp07621h2.cif
_cod_data_source_block           3719
_cod_depositor_comments
;Adding full bibliography for 7224460.cif.

 Adding full bibliography for 7224460.cif.
;
_cod_database_code               7224460
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C97E) \\sim Ueq, Uanis(C96E) \\sim Ueq, Uanis(C95E) \\sim Ueq,
Uanis(C90B) \\sim Ueq, Uanis(C92B) \\sim Ueq, Uanis(C93B) \\sim Ueq, Uanis(F6A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O7H) \\sim Ueq, Uanis(C96A) \\sim Ueq, Uanis(F6B) \\sim Ueq, Uanis(F4B)
\\sim Ueq, Uanis(F5A) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(F5A) \\sim Ueq, Uanis(O7B) \\sim Ueq, Uanis(O7C) \\sim Ueq, Uanis(O7F)
\\sim Ueq, Uanis(O7H) \\sim Ueq, Uanis(F3D) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C89A(H89A,H89B), C90A(H90A,H90B), C91A(H91A,H91B), C92A(H92A,H92B), C93A(H93A,
 H93B), C94A(H94A,H94B), C89B(H89C,H89D), C90B(H90C,H90D), C91B(H91C,H91D),
 C92B(H92C,H92D), C93B(H93C,H93D), C94B(H94C,H94D)
3.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C7A(H7A), C9A(H9A), C12A(H12A),
 C13A(H13A), C14A(H14A), C15A(H15A), C17A(H17A), C18A(H18A), C20A(H20A),
 C21A(H21A), C25A(H25A), C26A(H26A), C28A(H28A), C29A(H29A), C31A(H31A),
 C32A(H32A), C34A(H34A), C35A(H35A), C40A(H40A), C46A(H46A), C47A(H47A),
 C48A(H48A), C49A(H49A), C51A(H51A), C53A(H53A), C56A(H56A), C57A(H57A),
 C58A(H58A), C59A(H59A), C61A(H61A), C62A(H62A), C64A(H64A), C65A(H65A),
 C69A(H69A), C70A(H70A), C72A(H72A), C73A(H73A), C75A(H75A), C76A(H76A),
 C78A(H78A), C79A(H79A), C84A(H84A), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B),
 C7B(H7B), C9B(H9B), C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B), C17B(H17B),
  C18B(H18B), C20B(H20B), C21B(H21B), C25B(H25B), C26B(H26B), C28B(H28B),
 C29B(H29B), C31B(H31B), C32B(H32B), C34B(H34B), C35B(H35B), C40B(H40B),
 C46B(H46B), C47B(H47B), C48B(H48B), C49B(H49B), C51B(H51B), C53B(H53B),
 C56B(H56B), C57B(H57B), C58B(H58B), C59B(H59B), C61B(H61B), C62B(H62B),
 C64B(H64B), C65B(H65B), C69B(H69B), C70B(H70B), C72B(H72B), C73B(H73B),
 C75B(H75B), C76B(H76B), C78B(H78B), C79B(H79B), C84B(H84B)
3.c Idealised Me refined as rotating group:
 C41A(H41A,H41B,H41C), C42A(H42A,H42B,H42C), C43A(H43A,H43B,H43C), C44A(H44A,
 H44B,H44C), C85A(H85A,H85B,H85C), C86A(H86A,H86B,H86C), C87A(H87A,H87B,H87C),
 C88A(H88A,H88B,H88C), C41B(H41D,H41E,H41F), C42B(H42D,H42E,H42F), C43B(H43D,
 H43E,H43F), C44B(H44D,H44E,H44F), C85B(H85D,H85E,H85F), C86B(H86D,H86E,H86F),
 C87B(H87D,H87E,H87F), C88B(H88D,H88E,H88F), C95A(H95A,H95B,H95C), C97A(H97A,
 H97B,H97C), C95B(H95D,H95E,H95F), C97B(H97D,H97E,H97F), C95C(H95G,H95H,H95I),
 C97C(H97G,H97H,H97I), C95D(H95J,H95K,H95L), C97D(H97J,H97K,H97L), C95E(H95M,
 H95N,H95O), C97E(H97M,H97N,H97O), C95F(H95P,H95Q,H95R), C97F(H97P,H97Q,H97R),
 C95G(H95S,H95T,H95U), C97G(H97S,H97T,H97U), C95H(H95V,H95W,H95X), C97H(H97V,
 H97W,H97X), C95I(H95Y,H,HA), C97I(H97Y,HB,HC)
;
_olex2_submission_special_instructions 'No special instructions were received'