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_7040612
_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
'C50 H47 Ag B2 N8 O9 Zn2, 2.5(C H4 O), (C H3 N O2)'
_chemical_formula_sum            'C53.5 H60 Ag B2 N9 O13.5 Zn2'
_chemical_formula_weight         1305.33
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-03-18
_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                90
_cell_angle_beta                 96.9179(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3180(2)
_cell_length_b                   19.2910(4)
_cell_length_c                   27.0609(5)
_cell_measurement_reflns_used    22299
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.7850
_cell_measurement_theta_min      4.2630
_cell_volume                     6383.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46094
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         73.083
_diffrn_reflns_theta_min         4.010
_exptl_absorpt_coefficient_mu    3.846
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.358
_exptl_crystal_description       needle
_exptl_crystal_F_000             2676
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.614
_refine_diff_density_min         -2.525
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         12520
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0833
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+55.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.1807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11432
_reflns_number_total             12520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02758j2.cif
_cod_data_source_block           10
_cod_depositor_comments
;Adding full bibliography for 7040612--7040615.cif.

 Adding full bibliography for 7040612--7040615.cif.
;
_cod_original_formula_sum        'C53.50 H60 Ag B2 N9 O13.50 Zn2'
_cod_database_code               7040612
_shelxl_version_number           2014-3
_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 C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O7S-C5S
 1.47 with sigma of 0.02
 C35-C34A
 2.5 with sigma of 0.02
 C35A-C34
 2.5 with sigma of 0.02
 O1S-C1S
 1.47 with sigma of 0.02
 O6S-C4S = O7S-C5S
 1.47 with sigma of 0.02
 O8S-C6S
 1.47 with sigma of 0.005
 N1SB-C0AA \\sim C0AA-N1SA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C34 \\sim C34A: 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
C36 \\sim C36A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C5S) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(C1S) \\sim Ueq, Uanis(O1S) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.016
Uanis(N2S) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(O2SB) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(N1SB) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(O5S) = Uanis(O4S)
Uanis(C4S) = Uanis(O6S)
4. Others
 Fixed Sof: C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C35(0.5) H35A(0.5)
 H35B(0.5) H35C(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) O1S(0.5) H1S(0.5)
 C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) O3SB(0.25) O2SB(0.25) N1SB(0.25)
 O2SA(0.25) N1SA(0.25) O3SA(0.25) O4S(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5)
 H3SC(0.5) O5S(0.5) O6S(0.5) H6S(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5)
 C0AA(0.5) H0AA(0.25) H0AB(0.25) H0AC(0.25) H0AD(0.25) H0AE(0.25) H0AF(0.25)
 N2S(0.5) C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5) C35A(0.5) H35D(0.5) H35E(0.5)
 H35F(0.5) C36A(0.5) H36D(0.5) H36E(0.5) H36F(0.5) O8S(0.5) H8S(0.5) C6S(0.5)
 H6SA(0.5) H6SB(0.5) H6SC(0.5)
 Fixed Uiso: O8S(0.08) C6S(0.08)
5.a Riding coordinates:
 O6S(H6S)
5.b Me refined with riding coordinates:
 C0AA(H0AA,H0AB,H0AC), C0AA(H0AD,H0AE,H0AF)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C8(H8), C15(H15), C17(H17), C19(H19), C20(H20),
 C27(H27), C29(H29), C31(H31), C32(H32), C38(H38), C39(H39), C41(H41), C42(H42),
  C45(H45), C46(H46), C48(H48), C49(H49)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C5S(H5SA,H5SB,H5SC), C1S(H1SA,H1SB,H1SC),
 C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC), C34A(H34D,H34E,H34F), C35A(H35D,H35E,
 H35F), C36A(H36D,H36E,H36F), C6S(H6SA,H6SB,H6SC)
5.e Idealised tetrahedral OH refined as rotating group:
 O7S(H7S), O1S(H1S), O8S(H8S)
;
_shelx_res_checksum              75211
_olex2_submission_special_instructions 'No special instructions were received'