Ethynide-stabilized high-nuclearity silver(I) sulfido molecular clusters assembled using organic sulfide precursors
Zi-Yi Chen; Dennis Y. S. Tam; Thomas C. W. Mak; Chem.Commun. 52 (2016) 6119–; doi:

data_7119047
_publ_section_title
;
 Ethynide-stabilized high-nuclearity silver(I) sulfido molecular clusters
 assembled using organic sulfide precursors
;
_journal_name_full               Chem.Commun.
_journal_page_first              6119
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
'Ag45 C192 O2 S6, Ag C4 N2 O2, 2(B F4), 2(C O), 8(O)'
_chemical_formula_sum            'C198 Ag46 B2 F8 N2 O14 S6'
_chemical_formula_weight         7958.00
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-17 deposited with the CCDC.
2016-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.808(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.8433(12)
_cell_length_b                   28.2030(16)
_cell_length_c                   23.1207(13)
_cell_measurement_reflns_used    9636
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.56
_cell_volume                     12819.3(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            610184
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.516
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7308
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         22516
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1229P)^2^+121.4380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2480
_reflns_number_gt                17738
_reflns_number_total             22516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc02631a3.cif
_cod_data_source_block           1a
_cod_database_code               7119047
_olex2_refinement_description
;
1. Restrained distances
 O8-C97
 1.6 with sigma of 0.02
 C69-C68
 1.46 with sigma of 0.02
 O5-C200
 1.6 with sigma of 0.02
 C36-C34
 2.57 with sigma of 0.04
 C36-C35
 2.57 with sigma of 0.04
 C34-C35
 2.57 with sigma of 0.04
 C71-C72
 2.57 with sigma of 0.04
 C70-C71
 2.57 with sigma of 0.04
 C70-C72
 2.57 with sigma of 0.04
 C10-C1C
 2.57 with sigma of 0.04
 C10-C1B
 2.57 with sigma of 0.04
 C1C-C1B
 2.57 with sigma of 0.04
 C54-C53
 2.57 with sigma of 0.04
 C52-C53
 2.57 with sigma of 0.04
 C52-C54
 2.57 with sigma of 0.04
 C42-C41
 2.57 with sigma of 0.04
 C41-C40
 2.57 with sigma of 0.04
 C42-C40
 2.57 with sigma of 0.04
 C98-C99
 2.57 with sigma of 0.04
 C99-C100
 2.57 with sigma of 0.04
 C98-C100
 2.57 with sigma of 0.04
 C23-C24
 2.57 with sigma of 0.04
 C24-C25
 2.57 with sigma of 0.04
 C23-C25
 2.57 with sigma of 0.04
 C84-C87 \\sim C84-C85 \\sim C86-C84
 with sigma of 0.02
 C81-C98 \\sim C81-C99 \\sim C81-C100
 with sigma of 0.02
 C30-C24 \\sim C30-C25
 with sigma of 0.02
 C69-C70 \\sim C69-C72 \\sim C71-C69
 with sigma of 0.02
 C10-C27 \\sim C27-C1C \\sim C1B-C27
 with sigma of 0.02
 C28-C15 \\sim C28-C13 \\sim C28-C14
 with sigma of 0.02
 Ag31-Ag24 \\sim Ag4-Ag12
 with sigma of 0.02
 Ag24-Ag45 \\sim Ag3-Ag12
 with sigma of 0.02
 Ag31-Ag1 \\sim Ag4-Ag1
 with sigma of 0.02
2. Restrained angles
 C72-C69-C71
 fixed at 45 with sigma of 0.02
 C72-C69-C71
 fixed at 60 with sigma of 0.02
3. Others
 1*[Sof(Ag42)]+1*[Sof(Ag22)]=1 with esd of 0
 1*[Sof(Ag52)]+1*[Sof(Ag38)]+1*[Sof(Ag11)]=1 with esd of 0
 1*[Sof(Ag19)]+1*[Sof(Ag53)]+1*[Sof(Ag37)]=1 with esd of 0
 1*[Sof(Ag15)]+1*[Sof(Ag26)]+1*[Sof(Ag48)]=1 with esd of 0
 1*[Sof(Ag48)]+1*[Sof(Ag26)]+1*[Sof(Ag15)]=1 with esd of 0
 1*[Sof(Ag39)]+1*[Sof(Ag10)]+1*[Sof(Ag51)]=1 with esd of 0
 1*[Sof(Ag25)]+1*[Sof(Ag47)]+1*[Sof(Ag16)]=1 with esd of 0
 1*[Sof(Ag29)]+1*[Sof(Ag50)]+1*[Sof(Ag7)]=1 with esd of 0
 1*[Sof(Ag30)]+1*[Sof(Ag9)]+1*[Sof(Ag49)]=1 with esd of 0
 Sof(Ag8)=1-FVAR(1)
 Sof(Ag40)=FVAR(1)
 Sof(Ag35)=1-FVAR(2)
 Sof(Ag20)=FVAR(2)
 Sof(Ag14)=1-FVAR(3)
 Sof(Ag28)=FVAR(3)
 Sof(Ag34)=1-FVAR(4)
 Sof(Ag21)=FVAR(4)
 Sof(Ag32)=1-FVAR(13)
 Sof(Ag6)=FVAR(13)
 Sof(Ag5)=1-FVAR(29)
 Sof(Ag33)=FVAR(29)
 Sof(Ag43)=1-FVAR(30)
 Sof(Ag17)=FVAR(30)
 Sof(Ag27)=1-FVAR(31)
 Sof(Ag13)=FVAR(31)
 Sof(Ag18)=1-FVAR(32)
 Sof(Ag36)=FVAR(32)
 Sof(Ag41)=1-FVAR(33)
 Sof(Ag23)=FVAR(33)
 Fixed Sof: Ag2(0.66667) Ag3(0.66667) Ag4(0.66667) Ag12(0.66667) Ag24(0.33333)
 Ag31(0.33333) Ag44(0.33333) Ag45(0.33333) C98(0.5) C99(0.5) C100(0.5)
 C101(0.5) C102(0.5) C103(0.5) Ag46(0.5) O5(0.5) O6(0.5) N1(0.5) C94(0.5)
 C95(0.5) N2(0.5) C96(0.5) C200(0.5)
4.a Fitted pentagon refined as free rotating group:
 N1(C94,C95,N2,C96)
;
_olex2_submission_special_instructions 'No special instructions were received'