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_7040614
_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
'0.5(C152 H121 Ag2 B4 N20 O18 Zn4), 1.5(C H3 N O2), 0.75(C H4 O)'
_chemical_formula_sum            'C78.25 H68.5 Ag B2 N11.5 O12.75 Zn2'
_chemical_formula_weight         1634.17
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2016-04-18
_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                67.658(2)
_cell_angle_beta                 78.0034(17)
_cell_angle_gamma                65.410(2)
_cell_formula_units_Z            2
_cell_length_a                   15.6943(3)
_cell_length_b                   17.8805(5)
_cell_length_c                   18.0418(4)
_cell_measurement_reflns_used    24020
_cell_measurement_temperature    140.0(1)
_cell_measurement_theta_max      29.0900
_cell_measurement_theta_min      3.9380
_cell_volume                     4250.73(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015a)'
_computing_structure_solution    'SHEXTL (Sheldrick, 2015b)'
_diffrn_ambient_temperature      140.00(10)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device_type  'Super Nova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55999
_diffrn_reflns_point_group_measured_fraction_full 0.824
_diffrn_reflns_point_group_measured_fraction_max 0.678
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.480
_diffrn_reflns_theta_min         3.597
_diffrn_source                   'micro-focus sealed X-ray tuve'
_diffrn_source_type              'SuperNova Mo X-ray Source'
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_primary    'pale yellow'
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       plate
_exptl_crystal_F_000             1675
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.176
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 9588 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2059
_refine_ls_number_reflns         32067
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+16.9104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.571
_reflns_Friedel_fraction_full    0.653
_reflns_Friedel_fraction_max     0.493
_reflns_number_gt                28082
_reflns_number_total             32067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02758j2.cif
_cod_data_source_block           12
_cod_depositor_comments
;Adding full bibliography for 7040612--7040615.cif.

 Adding full bibliography for 7040612--7040615.cif.
;
_cod_original_cell_volume        4250.72(19)
_cod_original_formula_sum        'C78.25 H68.50 Ag B2 N11.50 O12.75 Zn2'
_cod_database_code               7040614
_shelxl_version_number           2014-3
_oxdiff_exptl_absorpt_empirical_full_min 0.523
_oxdiff_exptl_absorpt_empirical_full_max 1.520
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_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, All O(H) groups
2. Restrained distances
 C3BA-C1G
 2.5 with sigma of 0.02
 C32-C34 = C32-C35
 1.5 with sigma of 0.02
 C34-C35
 2.5 with sigma of 0.02
 C33-C32
 1.5 with sigma of 0.02
 C34-C33
 2.5 with sigma of 0.02
 C33-C35
 2.5 with sigma of 0.02
 C34-C27
 2.5 with sigma of 0.02
 O2S-O1S
 2 with sigma of 0.02
 O0AA-C16S
 1.47 with sigma of 0.02
 O12S-O11S
 2 with sigma of 0.02
 N9S-C9S
 1.4 with sigma of 0.02
 O15S-O14S = O1AA-O18S
 2.2 with sigma of 0.02
 N10S-C10S
 1.4 with sigma of 0.02
 H26-H35A
 2.15 with sigma of 0.01
 H26-H35E
 2.15 with sigma of 0.01
 C35A-C32
 1.5 with sigma of 0.02
 O14S-C9S \\sim C9S-O15S
 with sigma of 0.02
 O18S-C10S \\sim C10S-O1AA
 with sigma of 0.02
 O18S-N10S \\sim O1AA-N10S
 with sigma of 0.02
 O11S-C6S \\sim C6S-O12S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C32 \\sim C32A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C35 \\sim C35A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C34 \\sim C34A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C33 \\sim C33A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of
0.008 and sigma for terminal atoms of 0.008
Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.008 and sigma for terminal atoms of 0.016
Uanis(O1S) \\sim Ueq, Uanis(O12S) \\sim Ueq, Uanis(N6S) \\sim Ueq, Uanis(C6S)
\\sim Ueq, Uanis(O11S) \\sim Ueq, Uanis(C4S) \\sim Ueq, Uanis(O8S) \\sim Ueq,
Uanis(O7S) \\sim Ueq, Uanis(N4S) \\sim Ueq, Uanis(C16S) \\sim Ueq, Uanis(O0AA)
\\sim Ueq, Uanis(N9S) \\sim Ueq, Uanis(O15S) \\sim Ueq, Uanis(O14S) \\sim Ueq,
Uanis(C10S) \\sim Ueq, Uanis(N10S) \\sim Ueq, Uanis(O1AA) \\sim Ueq,
Uanis(O18S) \\sim Ueq, Uanis(O4S) \\sim Ueq, Uanis(O3S) \\sim Ueq: with sigma
of 0.006 and sigma for terminal atoms of 0.006
Uanis(C2S) \\sim Ueq, Uanis(C9S) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
Uanis(O2S) \\sim Ueq, Uanis(N1S) \\sim Ueq: with sigma of 0.006 and sigma for
terminal atoms of 0.006
Uiso(C23) = Uiso(C22A)
Uiso(C22) = Uiso(C21A)
Uiso(C21) = Uiso(C23A)
Uiso(C147) = Uiso(C1G)
Uiso(C3BA) = Uiso(C3BB)
Uiso(C0AA) = Uiso(C1H)
Uiso(C7AA) = Uiso(C74A)
Uiso(C9AA) = Uiso(C75A)
Uiso(C1BA) = Uiso(C73A)
Uiso(C0BA) = Uiso(C72A)
Uiso(C80) = Uiso(C66A)
Uiso(C79) = Uiso(C67A)
Uiso(C78) = Uiso(C68A)
Uiso(C6AA) = Uiso(C1I)
Uiso(N18) = Uiso(N18A)
4. Rigid body (RIGU) restrains
 C27, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C32(0.5) N18(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5)
 C0BA(0.5) C1BA(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C1G(0.5) H1GA(0.5) H1GB(0.5)
 H1GC(0.5) C3BA(0.5) H3BA(0.5) H3BB(0.5) H3BC(0.5) C6AA(0.5) C7AA(0.5)
 H7AA(0.5) H7AB(0.5) H7AC(0.5) C9AA(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5) C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5) C23(0.5)
 H23A(0.5) H23B(0.5) H23C(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5)
 H34A(0.5) H34B(0.5) H34C(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C78(0.5)
 H78(0.5) C79(0.5) C80(0.5) H80(0.5) N18A(0.5) C1H(0.5) H1HA(0.5) H1HB(0.5)
 H1HC(0.5) C1I(0.5) C3BB(0.5) H3BD(0.5) H3BE(0.5) H3BF(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C22A(0.5) H22D(0.5) H22E(0.5) H22F(0.5) C23A(0.5)
 H23D(0.5) H23E(0.5) H23F(0.5) C66A(0.5) H66A(0.5) C67A(0.5) C68A(0.5)
 H68A(0.5) C72A(0.5) C73A(0.5) H73A(0.5) H73B(0.5) H73C(0.5) C74A(0.5)
 H74A(0.5) H74B(0.5) H74C(0.5) C75A(0.5) H75A(0.5) H75B(0.5) H75C(0.5)
 C147(0.5) H14A(0.5) H14B(0.5) H14C(0.5) O3S(0.5) O2S(0.5) O1S(0.5) O4S(0.5)
 N2S(0.5) N1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) H2SC(0.5) N4S(0.5) O8S(0.5) O7S(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5)
 H4SC(0.5) N6S(0.5) O11S(0.5) O12S(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5)
 N10S(0.5) N9S(0.5) O1AA(0.5) O14S(0.5) O18S(0.5) O15S(0.5) C9S(0.5) H9SA(0.5)
 H9SB(0.5) H9SC(0.5) C10S(0.5) H10M(0.5) H10N(0.5) H10O(0.5) O0AA(0.5)
 H0AD(0.5) C16S(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C32A(0.5) C35A(0.5)
 H35D(0.5) H35E(0.5) H35F(0.5) C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5)
 C33A(0.5) H33D(0.5) H33E(0.5) H33F(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C8(H8), C15(H15), C17(H17), C19(H19), C20(H20),
 C26(H26), C30(H30), C31(H31), C37(H37), C39(H39), C41(H41), C43(H43), C44(H44),
  C46(H46), C47(H47), C50(H50), C51(H51), C53(H53), C54(H54), C57(H57),
 C59(H59), C61(H61), C63(H63), C64(H64), C66(H66), C67(H67), C70(H70), C71(H71),
  C73(H73), C74(H74), C82(H82), C83(H83), C86(H86), C88(H88), C90(H90),
 C91(H91), C96(H96), C98(H98), C100(H100), C101(H101), C107(H107), C109(H109),
 C111(H111), C113(H113), C114(H114), C116(H116), C117(H117), C120(H120),
 C121(H121), C123(H123), C124(H124), C126(H126), C128(H128), C130(H130),
 C132(H132), C133(H133), C135(H135), C136(H136), C139(H139), C140(H140),
 C142(H142), C143(H143), C78(H78), C80(H80), C66A(H66A), C68A(H68A)
6.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C103(H10D,H10E,
 H10F), C104(H10G,H10H,H10I), C105(H10J,H10K,H10L), C0AA(H0AA,H0AB,H0AC),
 C1BA(H1BA,H1BB,H1BC), C1G(H1GA,H1GB,H1GC), C3BA(H3BA,H3BB,H3BC), C7AA(H7AA,
 H7AB,H7AC), C9AA(H9AA,H9AB,H9AC), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F),
 C23(H23A,H23B,H23C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C1H(H1HA,H1HB,H1HC), C3BB(H3BD,H3BE,H3BF), C22(H22A,H22B,H22C),
 C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), C73A(H73A,H73B,H73C), C74A(H74A,
 H74B,H74C), C75A(H75A,H75B,H75C), C147(H14A,H14B,H14C), C1S(H1SA,H1SB,H1SC),
 C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC), C8S(H8SA,H8SB,H8SC), C6S(H6SA,H6SB,
 H6SC), C9S(H9SA,H9SB,H9SC), C10S(H10M,H10N,H10O), C16S(H16A,H16B,H16C),
 C35A(H35D,H35E,H35F), C34A(H34D,H34E,H34F), C33A(H33D,H33E,H33F)
6.c Idealised tetrahedral OH refined as rotating group:
 O13S(H13S), O0AA(H0AD)
;
_shelx_res_checksum              56387
_olex2_submission_special_instructions 'No special instructions were received'