Monitoring the Growth of Ag-S Clusters through Crystallization of Intermediate Clusters
Nan, Zi-Ang; Xiao, Ying; Liu, Xiyan; Wang, Tan; Cheng, Xiaoling; Yang, Yang; Lei, Zhen; Wang, Quan-Ming; Chemical Communications  (2019) –; doi:10.1039/C9CC03533H

data_7123458
_publ_section_title
;
 Monitoring the Growth of Ag-S Clusters through Crystallization of
 Intermediate Clusters
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03533H
_journal_year                    2019
_chemical_formula_moiety
'Ag45 C109.5 F21 O14 S31, 1.5(C2 N), 0.5(C O), 0.5(C3 N O)'
_chemical_formula_sum            'C117 H201 Ag45 F21 N3 O16 S31'
_chemical_formula_weight         8152.81
_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'
_audit_creation_date             2015-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2019-03-31 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.408(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3710(4)
_cell_length_b                   42.2618(11)
_cell_length_c                   26.5893(8)
_cell_measurement_temperature    100(2)
_cell_volume                     21337.4(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            99905
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.302
_exptl_absorpt_coefficient_mu    4.383
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61578
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.538
_exptl_crystal_description       plate
_exptl_crystal_F_000             15408
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.398
_refine_diff_density_min         -2.776
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2051
_refine_ls_number_reflns         37485
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+50.2949P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25318
_reflns_number_total             37485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03533h2.cif
_cod_data_source_block           p_CCDC2
_cod_database_code               7123458
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Restrained distances
 N21-C29 = N100-C52
 1.145 with sigma of 0.05
 C29-C5AA = C52-C60
 1.697 with sigma of 0.05
 N21-C5AA = N100-C60
 2.842 with sigma of 0.05
2. Rigid bond restraints
 C45, S23, Ag31, Ag43, Ag14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C20, C34, C33, C21, S17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C80B \\sim C57 \\sim C81 \\sim C82 \\sim S26: within 1.7A with sigma of 0.002
and sigma for terminal atoms of 0.005
C53B \\sim C94 \\sim C93 \\sim C54 \\sim S14 \\sim Ag37 \\sim Ag36 \\sim Ag30
\\sim Ag17: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
: with sigma of 0.005 and sigma for terminal atoms of 0.01
: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(C16)=1-FVAR(1)
 Sof(C1B)=FVAR(1)
 Sof(C1A)=1-FVAR(2)
 Sof(C1C)=FVAR(2)
 Sof(C99B)=1-FVAR(3)
 Sof(C99A)=FVAR(3)
 Sof(C53B)=1-FVAR(4)
 Sof(C53A)=FVAR(4)
 Sof(C44B)=1-FVAR(5)
 Sof(C44A)=FVAR(5)
 Fixed Sof: Ag15(0.75) Ag20(0.75) C95(0.5) C98(0.5) C90B(0.5) C97(0.5)
 C96(0.5) C91B(0.5) C300(0.5) C303(0.5) C301(0.5) C302(0.5) C5AA(0.5) N21(0.5)
 C29(0.5) O3AA(0.5) O48(0.5) C52(0.5) C60(0.5) C4AA(0.5) C3AA(0.5) N100(0.5)
 C7(0.5) C500(0.5) C22(0.5) C24(0.5) C142(0.5) C154(0.5) C182(0.5) C68(0.5)
 C73(0.5) Ag0A(0.25) Ag1A(0.25)
;
_shelx_res_checksum              4721
_olex2_submission_special_instructions 'No special instructions were received'