Assembly of high-symmetry silver(I) alkyl-1,3-diynyl cluster complexes via core transformation
Hau, Sam Chunkit; Mak, Thomas C. W.; Dalton Trans.  (2017) –; doi:10.1039/C7DT03406G

data_7044369
_publ_section_title
;
 Assembly of high-symmetry silver(I) alkyl-1,3-diynyl cluster complexes
 via core transformation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03406G
_journal_year                    2017
_chemical_formula_moiety         '2(C112 H80 Ag4 P4), 3(C2 H3 N)'
_chemical_formula_sum            'C230 H169 Ag8 N3 P8'
_chemical_formula_weight         4085.39
_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   geom
_audit_creation_date             2017-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-25 deposited with the CCDC.
2017-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3046(11)
_cell_length_b                   34.222(2)
_cell_length_c                   17.6558(11)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.943
_cell_measurement_theta_min      2.362
_cell_volume                     9633.8(10)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       APEX2(Bruker,2003)
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1147
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            173520
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.321
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  0.6082
_exptl_absorpt_correction_T_min  0.5028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1556 before and 0.1362 after correction. The Ratio of minimum to maximum transmission is 0.8267. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4132
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1146
_refine_ls_number_reflns         17458
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0733P)^2^+16.5707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14051
_reflns_number_total             17458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03406g2.cif
_cod_data_source_block           8
_cod_original_cell_volume        9633.8(11)
_cod_database_code               7044369
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.657
_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
2. Restrained distances
 C115-C116
 1.43 with sigma of 0.01
 C11-C12
 1.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: Ag4(0.9) Ag4'(0.1) C115(0.5) C116(0.5) H11D(0.5) H11E(0.5)
 H11F(0.5) N2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C36(H36),
  C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54),
  C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62),
 C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72),
  C73(H73), C74(H74), C75(H75), C76(H76), C78(H78), C79(H79), C80(H80),
 C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C90(H90),
  C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97), C98(H98),
 C99(H99), C100(H100), C102(H102), C103(H103), C104(H104), C105(H105),
 C106(H106), C108(H108), C109(H109), C110(H110), C111(H111), C112(H112)
5.b Idealised Me refined as rotating group:
 C114(H11A,H11B,H11C), C116(H11D,H11E,H11F)
;
_olex2_submission_special_instructions 'No special instructions were received'