#------------------------------------------------------------------------------
#$Date: 2016-01-09 12:32:52 +0200 (Sat, 09 Jan 2016) $
#$Revision: 173758 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/29/7222999.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7222999
loop_
_publ_author_name
'Yu, Tanlai'
'Fu, Yangbo'
'Wang, Yilin'
'Hao, Pengfei'
'Shen, Junju'
'Fu, Yunlong'
_publ_section_title
;
 Hierarchical symmetry transfer and flexible charge matching in five
 [M(phen)3]2+directed iodoargentates with 1 to 3D frameworks
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              8752
_journal_paper_doi               10.1039/C5CE01692D
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'Ag11 I15, 2(C36 H24 Co N6), H2 O'
_chemical_formula_sum            'C72 H50 Ag11 Co2 I15 N12 O'
_chemical_formula_weight         4307.17
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-10-04 deposited with the CCDC.
2015-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.8002(16)
_cell_length_b                   14.8002(16)
_cell_length_c                   24.789(3)
_cell_measurement_reflns_used    3269
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4480
_cell_measurement_theta_min      2.8710
_cell_volume                     4702.5(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0710
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10059
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_min         2.752
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.547
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    3.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         3.343
_refine_diff_density_min         -9.947
_refine_diff_density_rms         0.579
_refine_ls_extinction_coef       0.000141(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3168
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.1329
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+1144.6693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2941
_refine_ls_wR_factor_ref         0.2981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2932
_reflns_number_total             3168
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01692d2.cif
_cod_data_source_block           yu
_cod_depositor_comments
'Adding full bibliography for 7222998--7223004.cif.'
_cod_original_cell_volume        4702.4(11)
_cod_database_code               7222999
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.314
_shelx_estimated_absorpt_t_max   0.550
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.47313(13) 0.33046(12) 0.7500 0.0348(5) Uani 1 2 d S T P A .
Ag2 Ag 0.36689(17) 0.08088(19) 0.7500 0.0348(6) Uani 0.6667 2 d S TU P A 1
Ag3 Ag 0.13520(12) 0.08739(11) 0.67330(6) 0.0271(4) Uani 0.6667 1 d . U P A 1
Ag2B Ag 0.4172(3) 0.1069(3) 0.7500 0.0376(12) Uani 0.3333 2 d S TU P A 2
Ag3B Ag 0.2176(3) 0.1298(3) 0.7500 0.0286(12) Uani 0.3333 2 d S TU P A 2
I1 I 0.49414(10) 0.52912(9) 0.7500 0.0304(3) Uani 1 2 d S T P A .
I2 I 0.6667 0.3333 0.73675(17) 0.0439(16) Uani 0.5 3 d S T P A .
I3 I 0.35591(6) 0.19257(6) 0.65994(3) 0.0257(2) Uani 1 1 d . . . . .
I4 I 0.0000 0.0000 0.58355(6) 0.0457(5) Uani 1 3 d S T P . .
I5 I 0.07944(10) 0.19569(9) 0.7500 0.0283(3) Uani 1 2 d S TU P . .
Co1 Co 0.3333 0.6667 0.53259(11) 0.0193(7) Uani 1 3 d S T P . .
N1 N 0.2847(7) 0.7581(8) 0.5768(4) 0.018(2) Uani 1 1 d . U . . .
N2 N 0.3968(7) 0.8060(7) 0.4832(4) 0.019(2) Uani 1 1 d . U . . .
C1 C 0.2348(9) 0.7371(10) 0.6245(5) 0.024(3) Uani 1 1 d . U . . .
H1A H 0.2281 0.6807 0.6444 0.029 Uiso 1 1 calc R U . . .
C2 C 0.1933(10) 0.7940(10) 0.6454(6) 0.031(3) Uani 1 1 d . U . . .
H2A H 0.1559 0.7743 0.6775 0.038 Uiso 1 1 calc R U . . .
C3 C 0.2091(10) 0.8853(10) 0.6164(6) 0.030(3) Uani 1 1 d . U . . .
H3A H 0.1861 0.9284 0.6307 0.036 Uiso 1 1 calc R U . . .
C4 C 0.2604(10) 0.9083(9) 0.5657(5) 0.025(3) Uani 1 1 d . U . . .
C5 C 0.2702(11) 0.9923(11) 0.5338(6) 0.033(3) Uani 1 1 d . U . . .
H5A H 0.2408 1.0322 0.5445 0.039 Uiso 1 1 calc R U . . .
C6 C 0.3270(9) 1.0127(9) 0.4849(5) 0.021(2) Uani 1 1 d . U . . .
H6A H 0.3363 1.0682 0.4635 0.025 Uiso 1 1 calc R U . . .
C7 C 0.3689(9) 0.9522(9) 0.4684(5) 0.023(3) Uani 1 1 d . U . . .
C8 C 0.4261(10) 0.9704(10) 0.4210(5) 0.028(3) Uani 1 1 d . U . . .
H8A H 0.4360 1.0257 0.3992 0.033 Uiso 1 1 calc R U . . .
C9 C 0.4674(9) 0.9127(9) 0.4053(5) 0.020(3) Uani 1 1 d . U . . .
H9A H 0.5065 0.9286 0.3738 0.024 Uiso 1 1 calc R U . . .
C10 C 0.4497(8) 0.8238(8) 0.4388(5) 0.017(2) Uani 1 1 d . U . . .
H10A H 0.4759 0.7809 0.4285 0.020 Uiso 1 1 calc R U . . .
C11 C 0.3562(8) 0.8665(8) 0.4983(5) 0.016(2) Uani 1 1 d . U . . .
C12 C 0.2977(9) 0.8409(9) 0.5488(5) 0.019(2) Uani 1 1 d . U . . .
O1W O 0.3333 0.6667 0.7500 0.16(3) Uani 1 6 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
I1 Ag1 I2 113.57(5) . 10_557
I1 Ag1 I2 113.57(5) . .
I2 Ag1 I2 13.18(17) 10_557 .
I1 Ag1 I3 116.56(6) . .
I2 Ag1 I3 109.68(9) 10_557 .
I2 Ag1 I3 99.34(8) . .
I1 Ag1 I3 116.56(6) . 10_557
I2 Ag1 I3 99.34(8) 10_557 10_557
I2 Ag1 I3 109.68(9) . 10_557
I3 Ag1 I3 99.01(5) . 10_557
I1 Ag1 Ag2B 171.61(12) . .
I2 Ag1 Ag2B 74.76(10) 10_557 .
I2 Ag1 Ag2B 74.76(10) . .
I3 Ag1 Ag2B 59.27(5) . .
I3 Ag1 Ag2B 59.27(5) 10_557 .
I1 Ag1 Ag2 160.43(9) . .
I2 Ag1 Ag2 85.87(7) 10_557 .
I2 Ag1 Ag2 85.87(7) . .
I3 Ag1 Ag2 54.62(3) . .
I3 Ag1 Ag2 54.62(3) 10_557 .
I1 Ag2 I3 124.29(6) 2_655 10_557
I1 Ag2 I3 124.29(6) 2_655 .
I3 Ag2 I3 104.13(10) 10_557 .
I1 Ag2 Ag1 126.69(9) 2_655 .
I3 Ag2 Ag1 57.74(5) 10_557 .
I3 Ag2 Ag1 57.74(5) . .
I1 Ag2 I5 109.05(8) 2_655 3
I3 Ag2 I5 92.78(6) 10_557 3
I3 Ag2 I5 92.78(6) . 3
Ag1 Ag2 I5 124.26(10) . 3
I4 Ag3 I3 120.86(6) . .
I4 Ag3 I5 116.20(7) . .
I3 Ag3 I5 110.13(5) . .
I4 Ag3 I5 111.45(5) . 3
I3 Ag3 I5 97.61(7) . 3
I5 Ag3 I5 96.02(5) . 3
I4 Ag3 Ag3 57.53(3) . 3
I3 Ag3 Ag3 138.42(10) . 3
I5 Ag3 Ag3 104.86(5) . 3
I5 Ag3 Ag3 56.35(5) 3 3
I4 Ag3 Ag3 57.53(3) . 2
I3 Ag3 Ag3 160.03(9) . 2
I5 Ag3 Ag3 61.33(7) . 2
I5 Ag3 Ag3 101.17(5) 3 2
Ag3 Ag3 Ag3 60.0 3 2
I1 Ag2B I3 129.67(8) 2_655 10_557
I1 Ag2B I3 129.67(8) 2_655 .
I3 Ag2B I3 99.44(17) 10_557 .
I1 Ag2B Ag1 150.69(18) 2_655 .
I3 Ag2B Ag1 59.58(9) 10_557 .
I3 Ag2B Ag1 59.58(9) . .
I1 Ag2B Ag3B 140.75(16) 2_655 .
I3 Ag2B Ag3B 56.00(10) 10_557 .
I3 Ag2B Ag3B 56.00(10) . .
Ag1 Ag2B Ag3B 68.56(14) . .
I5 Ag3B I5 109.49(14) . 3
I5 Ag3B I3 115.91(13) . 10_557
I5 Ag3B I3 105.79(14) 3 10_557
I5 Ag3B I3 115.91(13) . .
I5 Ag3B I3 105.80(14) 3 .
I3 Ag3B I3 103.01(13) 10_557 .
I5 Ag3B Ag2B 166.90(17) . .
I5 Ag3B Ag2B 83.62(17) 3 .
I3 Ag3B Ag2B 58.26(9) 10_557 .
I3 Ag3B Ag2B 58.26(9) . .
Ag2B I1 Ag1 80.92(10) 3_665 .
Ag1 I1 Ag2 93.74(7) . 3_665
I2 I2 Ag1 83.41(8) 10_557 .
I2 I2 Ag1 83.42(8) 10_557 2_655
Ag1 I2 Ag1 118.70(3) . 2_655
I2 I2 Ag1 83.41(8) 10_557 3_665
Ag1 I2 Ag1 118.70(3) . 3_665
Ag1 I2 Ag1 118.70(3) 2_655 3_665
Ag2 I3 Ag3 88.52(6) . .
Ag3B I3 Ag2B 65.74(13) . .
Ag2 I3 Ag1 67.65(5) . .
Ag3 I3 Ag1 114.15(5) . .
Ag3B I3 Ag1 73.13(7) . .
Ag2B I3 Ag1 61.15(8) . .
Ag3 I4 Ag3 64.94(6) 2 3
Ag3 I4 Ag3 64.94(6) 2 .
Ag3 I4 Ag3 64.94(6) 3 .
Ag3B I5 Ag3B 130.51(14) . 2
Ag3 I5 Ag3 83.28(8) . 10_557
Ag3 I5 Ag3 62.32(6) . 2
Ag3 I5 Ag3 111.91(6) 10_557 2
Ag3 I5 Ag3 111.91(6) . 11_557
Ag3 I5 Ag3 62.32(6) 10_557 11_557
Ag3 I5 Ag3 78.16(7) 2 11_557
Ag3 I5 Ag2 134.74(5) . 2
Ag3 I5 Ag2 134.74(5) 10_557 2
Ag3 I5 Ag2 78.32(6) 2 2
Ag3 I5 Ag2 78.32(6) 11_557 2
N1 Co1 N1 95.8(4) . 2_665
N1 Co1 N1 95.8(4) . 3_565
N1 Co1 N1 95.8(4) 2_665 3_565
N1 Co1 N2 168.6(4) . 3_565
N1 Co1 N2 94.8(4) 2_665 3_565
N1 Co1 N2 79.0(4) 3_565 3_565
N1 Co1 N2 79.0(4) . .
N1 Co1 N2 168.6(4) 2_665 .
N1 Co1 N2 94.8(4) 3_565 .
N2 Co1 N2 91.2(4) 3_565 .
N1 Co1 N2 94.8(4) . 2_665
N1 Co1 N2 79.0(4) 2_665 2_665
N1 Co1 N2 168.6(4) 3_565 2_665
N2 Co1 N2 91.2(4) 3_565 2_665
N2 Co1 N2 91.2(4) . 2_665
C12 N1 C1 118.7(13) . .
C12 N1 Co1 112.1(8) . .
C1 N1 Co1 128.8(10) . .
C10 N2 C11 121.5(11) . .
C10 N2 Co1 127.0(10) . .
C11 N2 Co1 110.3(7) . .
N1 C1 C2 123.6(13) . .
N1 C1 H1A 118.2 . .
C2 C1 H1A 118.2 . .
C1 C2 C3 118.4(13) . .
C1 C2 H2A 120.8 . .
C3 C2 H2A 120.8 . .
C4 C3 C2 118.8(15) . .
C4 C3 H3A 120.6 . .
C2 C3 H3A 120.6 . .
C5 C4 C3 120.8(15) . .
C5 C4 C12 123.0(12) . .
C3 C4 C12 116.2(13) . .
C4 C5 C6 116.9(15) . .
C4 C5 H5A 121.5 . .
C6 C5 H5A 121.5 . .
C7 C6 C5 121.7(13) . .
C7 C6 H6A 119.2 . .
C5 C6 H6A 119.2 . .
C6 C7 C8 123.4(13) . .
C6 C7 C11 122.0(12) . .
C8 C7 C11 114.5(14) . .
C9 C8 C7 123.5(13) . .
C9 C8 H8A 118.2 . .
C7 C8 H8A 118.2 . .
C8 C9 C10 118.4(11) . .
C8 C9 H9A 120.8 . .
C10 C9 H9A 120.8 . .
N2 C10 C9 118.7(13) . .
N2 C10 H10A 120.6 . .
C9 C10 H10A 120.6 . .
N2 C11 C7 123.3(11) . .
N2 C11 C12 117.8(11) . .
C7 C11 C12 118.9(13) . .
N1 C12 C4 124.2(11) . .
N1 C12 C11 118.6(13) . .
C4 C12 C11 117.2(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 I1 2.798(2) .
Ag1 I2 2.862(2) 10_557
Ag1 I2 2.862(2) .
Ag1 I3 2.9356(12) .
Ag1 I3 2.9356(12) 10_557
Ag1 Ag2B 2.982(5) .
Ag1 Ag2 3.211(3) .
Ag2 I1 2.819(3) 2_655
Ag2 I3 2.830(2) 10_557
Ag2 I3 2.830(2) .
Ag2 I5 3.254(3) 3
Ag3 I4 2.8352(19) .
Ag3 I3 2.8493(17) .
Ag3 I5 2.862(2) .
Ag3 I5 3.0163(18) 3
Ag3 Ag3 3.044(2) 3
Ag3 Ag3 3.044(2) 2
Ag2B I1 2.591(6) 2_655
Ag2B I3 2.926(4) 10_557
Ag2B I3 2.926(4) .
Ag2B Ag3B 3.137(8) .
Ag3B I5 2.670(6) .
Ag3B I5 2.682(5) 3
Ag3B I3 2.852(3) 10_557
Ag3B I3 2.852(3) .
I1 Ag2B 2.591(6) 3_665
I1 Ag2 2.819(3) 3_665
I2 I2 0.657(8) 10_557
I2 Ag1 2.862(2) 2_655
I2 Ag1 2.862(2) 3_665
I4 Ag3 2.8352(19) 2
I4 Ag3 2.8352(19) 3
I5 Ag3B 2.682(5) 2
I5 Ag3 2.862(2) 10_557
I5 Ag3 3.0163(19) 2
I5 Ag3 3.0163(19) 11_557
I5 Ag2 3.254(3) 2
Co1 N1 2.128(12) .
Co1 N1 2.128(12) 2_665
Co1 N1 2.128(12) 3_565
Co1 N2 2.168(10) 3_565
Co1 N2 2.168(10) .
Co1 N2 2.168(10) 2_665
N1 C12 1.336(17) .
N1 C1 1.345(16) .
N2 C10 1.299(15) .
N2 C11 1.357(19) .
C1 C2 1.37(2) .
C1 H1A 0.9300 .
C2 C3 1.44(2) .
C2 H2A 0.9300 .
C3 C4 1.419(19) .
C3 H3A 0.9300 .
C4 C5 1.42(2) .
C4 C12 1.42(2) .
C5 C6 1.418(19) .
C5 H5A 0.9300 .
C6 C7 1.38(2) .
C6 H6A 0.9300 .
C7 C8 1.395(19) .
C7 C11 1.397(18) .
C8 C9 1.33(2) .
C8 H8A 0.9300 .
C9 C10 1.465(18) .
C9 H9A 0.9300 .
C10 H10A 0.9300 .
C11 C12 1.461(16) .
