Mechanical switching of magnetic interaction by tweezers-type complex.
Doistau, Benjamin; Cantin, Jean-Louis; Chamoreau, Lise-Marie; Marvaud, Valérie; Hasenknopf, Bernold; Vives, Guillaume; Chemical communications (Cambridge, England) 51 (2015) 12916–12919; doi:10.1039/c5cc04980f

data_7117607
_publ_section_title
;
 Mechanical switching of magnetic interaction by tweezers-type complex.
;
_journal_issue                   65
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12916
_journal_page_last               12919
_journal_paper_doi               10.1039/c5cc04980f
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C91 H98 Cl2 Cu2 N7 O4 Zn, 3(C H Cl3)'
_chemical_formula_sum            'C94 H101 Cl11 Cu2 N7 O4 Zn'
_chemical_formula_weight         1975.21
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2014-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_audit_update_record
;
2015-03-04 deposited with the CCDC.
2015-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.123(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   69.071(3)
_cell_length_b                   14.7327(6)
_cell_length_c                   19.7966(8)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    200
_cell_measurement_theta_max      69.87
_cell_measurement_theta_min      4.74
_cell_volume                     19943.0(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker QUAZAR'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       77
_diffrn_reflns_limit_h_min       -84
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84593
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.156
_diffrn_reflns_theta_min         2.585
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.884
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1251 before and 0.0525 after correction.
The Ratio of minimum to maximum transmission is 0.6428.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             8168
_exptl_crystal_preparation       CHCl3
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.836
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         18504
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1098P)^2^+79.7007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1985
_refine_ls_wR_factor_ref         0.2079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15500
_reflns_number_total             18504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc04980f2.cif
_cod_data_source_block           bd251114_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_cell_volume        19942.9(14)
_cod_database_code               7117607
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C96A-Cl13 = C96A-Cl14 = C96A-Cl15
 1.79 with sigma of 0.02
 C96B-Cl16 = C96B-Cl17 = C96B-Cl18
 1.79 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C96A \\sim Cl13 \\sim Cl14 \\sim Cl15: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C96B \\sim Cl16 \\sim Cl17 \\sim Cl18: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C96A, Cl13, Cl14, Cl15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C96B, Cl16, Cl17, Cl18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C93(0.5) H93(0.5) C94(0.5) H94(0.5) C95(0.5) H95(0.5) Cl10(0.5)
 Cl11(0.5) Cl12(0.5) C96A(0.25) H96A(0.25) Cl13(0.25) Cl14(0.25) Cl15(0.25)
 C96B(0.25) H96B(0.25) Cl16(0.25) Cl17(0.25) Cl18(0.25)
6.a Ternary CH refined with riding coordinates:
 C92(H92), C93(H93), C94(H94), C95(H95), C96A(H96A), C96B(H96B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C15(H15), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24),
 C26(H26), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C47(H47), C50(H50),
  C51(H51), C52(H52), C57(H57), C58(H58), C61(H61), C62(H62), C64(H64),
 C66(H66), C79(H79), C81(H81)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C),
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C85(H85A,H85B,
 H85C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C), C90(H90A,
 H90B,H90C), C91(H91A,H91B,H91C)
;
_shelx_res_checksum              7959
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'