Dinuclear clathrochelate complexes with pendent cyano groups as metalloligands.
Marmier, Mathieu; Cecot, Giacomo; Vologzhanina, Anna V.; Bila, José L; Zivkovic, Ivica; Ronnow, Henrik M.; Nafradi, Balint; Solari, Euro; Pattison, Philip; Scopelliti, Rosario; Severin, Kay; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15507–15516; doi:10.1039/c6dt02758j

data_7040615
_publ_section_title
;
 Dinuclear clathrochelate complexes with pendent cyano groups as
 metalloligands.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15507
_journal_page_last               15516
_journal_paper_doi               10.1039/c6dt02758j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C118 H64 Ag3 B4 Co4 N22 O18, C6 H4 Cl2, C H3 O'
_chemical_formula_sum            'C125 H71 Ag3 B4 Cl2 Co4 N22 O19'
_chemical_formula_weight         2858.50
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-20 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.6211(2)
_cell_length_b                   14.72200(10)
_cell_length_c                   34.9798(3)
_cell_measurement_reflns_used    37196
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      1.50
_cell_measurement_theta_min      22.75
_cell_volume                     20918.8(3)
_computing_cell_refinement
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)'
_computing_data_collection
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_solution    Sir2014
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.680
_diffrn_measured_fraction_theta_max 0.829
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69710
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.680
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            89199
_diffrn_reflns_point_group_measured_fraction_full 0.680
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        24.725
_diffrn_reflns_theta_max         23.036
_diffrn_reflns_theta_min         1.507
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'orange clear'
_exptl_crystal_colour_primary    'orange clear'
_exptl_crystal_density_diffrn    0.908
_exptl_crystal_description       needle
_exptl_crystal_F_000             5720
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.31(3)
_refine_ls_extinction_coef       0.00062(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1558
_refine_ls_number_reflns         25055
_refine_ls_number_restraints     397
_refine_ls_restrained_S_all      1.290
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2042
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_full    0.681
_reflns_Friedel_fraction_max     0.832
_reflns_number_gt                21882
_reflns_number_total             25055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02758j2.cif
_cod_data_source_block           13
_cod_depositor_comments
;Adding full bibliography for 7040612--7040615.cif.

 Adding full bibliography for 7040612--7040615.cif.
;
_cod_database_code               7040615
_shelxl_version_number           2014-3
_oxdiff_exptl_absorpt_empirical_full_min 0.633
_oxdiff_exptl_absorpt_empirical_full_max 1.823
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.69(3) 0.31(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O2S-C14S
 1.4 with sigma of 0.02
 O1S-C13S
 1.4 with sigma of 0.02
 O1S-Ag2 \\sim Ag2-O2S
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Ag2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(C3S) \\sim Ueq, Uanis(C5S) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(N20) \\sim Ueq: with sigma of 0.006 and
sigma for terminal atoms of 0.006
Uanis(C11S) \\sim Ueq, Uanis(N21) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.006 and sigma for terminal
atoms of 0.006
Uanis(C70) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C88)
\\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.006 and
sigma for terminal atoms of 0.006
Uanis(C104) = Uanis(C106) = Uanis(C105) = Uanis(C107) = Uanis(C109) =
Uanis(C108)
Uanis(C53) = Uanis(C54) = Uanis(C55) = Uanis(C56) = Uanis(C57) = Uanis(C58) =
Uanis(C59)
5. Rigid body (RIGU) restrains
 C114, C115, C113, C116, N19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2AA, C1A, C101, C100
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C102, C103, C99, C1A, N22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C50, C49, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8S, C9S, C10S, C11S, C12S, C7S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1S, C2S, C3S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C52, C46, C47, C48, C49, C50, N7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27, C28, C30, N10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C42, C43, C45, N11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C69, C70, C71, C74, N20, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, C59, C57, C58, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C83, C84, C85, C78, C88
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C47, C46, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl3S(0.5) Cl4S(0.5) C11S(0.5) H11S(0.5) C12S(0.5) H12S(0.5)
 C7S(0.5) C8S(0.5) C9S(0.5) H9S(0.5) C10S(0.5) H10S(0.5) Cl1S(0.5) Cl2S(0.5)
 C3S(0.5) H3S(0.5) C2S(0.5) C1S(0.5) C6S(0.5) H6S(0.5) C5S(0.5) H5S(0.5)
 C4S(0.5) H4S(0.5) O1S(0.5) O2S(0.5) C13S(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
 C14S(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 Fixed Uiso: C13S(0.1) C14S(0.1)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C18(H18), C20(H20), C22(H22), C23(H23), C25(H25), C29(H29), C28(H28), C26(H26),
  C33(H33), C35(H35), C37(H37), C38(H38), C40(H40), C41(H41), C43(H43),
 C44(H44), C51(H51), C50(H50), C48(H48), C47(H47), C54(H54), C55(H55), C57(H57),
  C58(H58), C62(H62), C64(H64), C66(H66), C67(H67), C69(H69), C70(H70),
 C72(H72), C73(H73), C77(H77), C79(H79), C81(H81), C82(H82), C84(H84), C85(H85),
  C87(H87), C88(H88), C92(H92), C94(H94), C96(H96), C97(H97), C99(H99),
 C100(H100), C1A(H1A), C2AA(H2AA), C104(H104), C105(H105), C107(H107),
 C108(H108), C111(H111), C112(H112), C114(H114), C115(H115), C11S(H11S),
 C12S(H12S), C9S(H9S), C10S(H10S), C3S(H3S), C6S(H6S), C5S(H5S), C4S(H4S)
7.b Fitted hexagon refined as free rotating group:
 C25(C24,C29,C28,C27,C26), C51(C50,C49,C48,C47,C46), C103(C104,C105,C106,C107,
 C108), C11S(C12S,C7S,C8S,C9S,C10S), C3S(C2S,C1S,C6S,C5S,C4S)
7.c Idealised Me refined as rotating group:
 C13S(H13A,H13B,H13C), C14S(H14A,H14B,H14C)
;
_shelx_res_checksum              98094
_shelx_fab_checksum              89358
_olex2_submission_special_instructions 'No special instructions were received'