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_7044367
_publ_section_title
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 Assembly of high-symmetry silver(I) alkyl-1,3-diynyl cluster complexes
 via core transformation
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_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03406G
_journal_year                    2017
_chemical_formula_moiety
'2(N O3), C204 H186 Ag8 P8, 8(C H4 O), 3(H2 O)'
_chemical_formula_sum            'C212 H224 Ag8 N2 O17 P8'
_chemical_formula_weight         4182.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 110.535(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.288(2)
_cell_length_b                   30.351(2)
_cell_length_c                   18.6689(12)
_cell_measurement_reflns_used    9677
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.40
_cell_volume                     19255(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1370
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            212944
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.777
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  27.94
_exptl_absorpt_correction_T_min  2.40
_exptl_absorpt_correction_type   multi-scan
_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    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             8568
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.244
_refine_diff_density_min         -1.301
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1102
_refine_ls_number_reflns         17402
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+59.6161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1433
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14287
_reflns_number_total             17402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03406g2.cif
_cod_data_source_block           1
_cod_database_code               7044367
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.769
_shelx_estimated_absorpt_t_min   0.655
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O2-N1
 1.43 with sigma of 0.02
 O3-N1
 1.43 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(O4)
\\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, :
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O2W(0.5) H2WA(0.5) H2WB(0.5)
5.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.b Ternary CH refined with riding coordinates:
 C5(H5), C15(H15), C25(H25)
5.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
5.d Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
  C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
 C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
  C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75),
 C76(H76), C77(H77), C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
  C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93),
 C94(H94), C95(H95), C96(H96), C98(H98), C99(H99), C100(H100), C101(H101),
 C102(H102)
5.e Idealised Me refined as rotating group:
 C103(H10C,H10D,H10E), C104(H10F,H10G,H10H), C105(H10I,H10J,H10K), C106(H10L,
 H10M,H10N)
5.f Idealised tetrahedral OH refined as rotating group:
 O4(H4), O5(H5A), O6(H6), O7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'