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_7040613
_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
'C51 H51 Ag B2 Co2 N8 O10, 1.25(C H4 O), 1.5(C H3 N O2)'
_chemical_formula_sum            'C53.75 H60.5 Ag B2 Co2 N9.5 O14.25'
_chemical_formula_weight         1314.96
_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             2016-03-17
_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                 97.324(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3035(11)
_cell_length_b                   19.295(4)
_cell_length_c                   27.164(3)
_cell_measurement_reflns_used    2135
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      3.15
_cell_volume                     6396.0(16)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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    'SHELXT (Sheldrick, 2015b)''
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            106504
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         3.099
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0628 before and 0.0542 after correction.
The Ratio of minimum to maximum transmission is 0.8592.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       needle
_exptl_crystal_F_000             2698
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.108
_refine_diff_density_min         -2.109
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         18526
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+33.2804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14988
_reflns_number_total             18526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02758j2.cif
_cod_data_source_block           11
_cod_depositor_comments
;Adding full bibliography for 7040612--7040615.cif.

 Adding full bibliography for 7040612--7040615.cif.
;
_cod_original_cell_volume        6395.9(15)
_cod_original_formula_sum        'C53.75 H60.50 Ag B2 Co2 N9.50 O14.25'
_cod_database_code               7040613
_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
 O10-H10
 0.87 with sigma of 0.01
 O7S-C5S
 1.47 with sigma of 0.02
 O6S-C4S
 1.47 with sigma of 0.02
 C51-H10
 1.924044 with sigma of 0.02
 Ag1-H10
 3.227168 with sigma of 0.02
 O5S-N2S \\sim O4S-N2S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1S) \\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.004
Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
Uanis(O4S) \\sim Ueq, Uanis(N2S) \\sim Ueq, Uanis(O5S) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.005
Uanis(O7S) = Uanis(C5S) = Uanis(O6S) = Uanis(C4S)
Uanis(O3SB) = Uanis(O2SB)
4. Others
 Fixed Sof: O1S(0.5) H1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) H2SA(0.5)
 H2SB(0.5) H2SC(0.5) H2SD(0.5) H2SE(0.5) H2SF(0.5) O3SB(0.5) O2SB(0.5)
 N1SB(0.5) O2SA(0.5) N1SA(0.5) O3SA(0.5) O4S(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5)
 H3SC(0.5) N2S(0.5) O5S(0.5) O6S(0.5) H6S(0.5) C5S(0.25) H5SA(0.25) H5SB(0.25)
 H5SC(0.25) O7S(0.25) H7S(0.25) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5)
5.a Riding coordinates:
 O7S(H7S)
5.b Me refined with riding coordinates:
 C2S(H2SA,H2SB,H2SC), C2S(H2SD,H2SE,H2SF)
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), C51(H51A,H51B,H51C), C1S(H1SA,H1SB,H1SC),
 C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC), C4S(H4SA,H4SB,H4SC)
5.e Idealised tetrahedral OH refined as rotating group:
 O1S(H1S), O6S(H6S)
;
_shelx_res_checksum              7114
_olex2_submission_special_instructions 'No special instructions were received'