#------------------------------------------------------------------------------
#$Date: 2019-11-23 09:29:26 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232720 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/80/4348067.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_4348067
loop_
_publ_author_name
'Hawes, Chris S.'
'Hamilton, Sophie E.'
'Hicks, Jamie'
'Knowles, Gregory P.'
'Chaffee, Alan L.'
'Turner, David R.'
'Batten, Stuart R.'
_publ_section_title
;
 Coordination Chemistry and Structural Dynamics of a Long and Flexible
 Piperazine-Derived Ligand.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6692
_journal_page_last               6702
_journal_paper_doi               10.1021/acs.inorgchem.6b00933
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C30 H36 Ag2 F6 N6 O6 S2'
_chemical_formula_sum            'C30 H36 Ag2 F6 N6 O6 S2'
_chemical_formula_weight         970.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                74.860(6)
_cell_angle_beta                 85.802(10)
_cell_angle_gamma                65.050(11)
_cell_formula_units_Z            1
_cell_length_a                   9.386(2)
_cell_length_b                   9.596(2)
_cell_length_c                   11.148(2)
_cell_measurement_reflns_used    18923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.50
_cell_measurement_theta_min      1.89
_cell_volume                     878.0(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18923
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.495
_diffrn_reflns_theta_min         1.895
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.039(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0610P)²+0.9250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3679
_reflns_number_total             4282
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b00933_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4348067
_shelxl_version_number           2014/6
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C17(H17), C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Ag1 Ag 0.46139(3) 0.71501(3) 0.35039(3) 0.02963(12) Uani 1 1 d .
N2 N -0.3014(3) 0.6935(3) 0.3644(3) 0.0269(6) Uani 1 1 d .
C3 C -0.1815(4) 0.5948(4) 0.3114(3) 0.0271(6) Uani 1 1 d .
H3 H -0.2020 0.5316 0.2682 0.033 Uiso 1 1 calc R
C4 C -0.0297(4) 0.5817(4) 0.3173(3) 0.0273(6) Uani 1 1 d .
H4 H 0.0515 0.5120 0.2774 0.033 Uiso 1 1 calc R
C5 C 0.0040(4) 0.6711(4) 0.3821(3) 0.0247(6) Uani 1 1 d .
C6 C -0.1209(4) 0.7715(4) 0.4385(3) 0.0294(7) Uani 1 1 d .
H6 H -0.1032 0.8336 0.4846 0.035 Uiso 1 1 calc R
C7 C -0.2694(4) 0.7801(4) 0.4272(4) 0.0311(7) Uani 1 1 d .
H7 H -0.3531 0.8501 0.4652 0.037 Uiso 1 1 calc R
C8 C 0.1691(4) 0.6558(4) 0.3955(3) 0.0266(6) Uani 1 1 d .
H8A H 0.1854 0.6612 0.4806 0.032 Uiso 1 1 calc R
H8B H 0.2436 0.5493 0.3870 0.032 Uiso 1 1 calc R
N9 N 0.2094(3) 0.7779(3) 0.3046(3) 0.0230(5) Uani 1 1 d .
C10 C 0.1123(4) 0.9399(4) 0.3179(3) 0.0248(6) Uani 1 1 d .
H10A H 0.1208 0.9432 0.4051 0.030 Uiso 1 1 calc R
H10B H 0.0007 0.9699 0.2974 0.030 Uiso 1 1 calc R
C11 C 0.1674(4) 1.0560(4) 0.2320(3) 0.0272(7) Uani 1 1 d .
H11A H 0.1030 1.1645 0.2419 0.033 Uiso 1 1 calc R
H11B H 0.2783 1.0273 0.2539 0.033 Uiso 1 1 calc R
N12 N 0.1535(4) 1.0535(3) 0.1025(3) 0.0279(6) Uani 1 1 d .
C13 C 0.2430(4) 0.8931(4) 0.0866(3) 0.0301(7) Uani 1 1 d .
H13A H 0.3565 0.8610 0.1018 0.036 Uiso 1 1 calc R
H13B H 0.2271 0.8923 0.0000 0.036 Uiso 1 1 calc R
C14 C 0.1919(4) 0.7751(4) 0.1757(3) 0.0270(6) Uani 1 1 d .
H14A H 0.0806 0.8021 0.1563 0.032 Uiso 1 1 calc R
H14B H 0.2566 0.6669 0.1653 0.032 Uiso 1 1 calc R
C15 C 0.2038(4) 1.1658(4) 0.0164(3) 0.0308(7) Uani 1 1 d .
H15A H 0.2067 1.1495 -0.0680 0.037 Uiso 1 1 calc R
H15B H 0.3119 1.1433 0.0414 0.037 Uiso 1 1 calc R
C16 C 0.0978(4) 1.3374(4) 0.0117(3) 0.0279(7) Uani 1 1 d .
C17 C -0.0625(4) 1.3884(4) 0.0292(3) 0.0293(7) Uani 1 1 d .
H17 H -0.1069 1.3130 0.0497 0.035 Uiso 1 1 calc R
C18 C 0.1585(4) 1.4523(4) -0.0171(3) 0.0297(7) Uani 1 1 d .
H18 H 0.2681 1.4202 -0.0285 0.036 Uiso 1 1 calc R
O19 O 0.5346(4) 0.4169(3) 0.3727(4) 0.0511(8) Uani 1 1 d .
S20 S 0.63226(10) 0.26379(10) 0.35244(9) 0.0333(2) Uani 1 1 d .
O21 O 0.6306(4) 0.1347(3) 0.4523(3) 0.0414(6) Uani 1 1 d .
O22 O 0.7835(3) 0.2463(4) 0.3069(3) 0.0487(7) Uani 1 1 d .
C23 C 0.5292(6) 0.2528(6) 0.2253(4) 0.0489(10) Uani 1 1 d .
F24 F 0.3798(4) 0.2818(4) 0.2526(3) 0.0650(8) Uani 1 1 d .
F25 F 0.5278(5) 0.3608(5) 0.1218(3) 0.0767(10) Uani 1 1 d .
F26 F 0.5982(5) 0.1117(4) 0.2008(3) 0.0708(9) Uani 1 1 d .
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'
Ag Ag -0.8740 1.0960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1240 0.1230 '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
N2 Ag1 N9 168.86(10) 1_655 .
N2 Ag1 O19 96.87(10) 1_655 .
N2 Ag1 O21 91.49(10) 1_655 2_666
N9 Ag1 O19 90.95(10) . .
N9 Ag1 O21 90.56(10) . 2_666
O19 Ag1 O21 124.67(10) . 2_666
C3 N2 Ag1 121.8(2) . 1_455
C3 N2 C7 117.8(3) . .
C7 N2 Ag1 120.4(2) . 1_455
N2 C3 H3 118.7 . .
N2 C3 C4 122.7(3) . .
C4 C3 H3 118.7 . .
C3 C4 H4 120.1 . .
C3 C4 C5 119.8(3) . .
C5 C4 H4 120.1 . .
C4 C5 C6 117.1(3) . .
C4 C5 C8 121.7(3) . .
C6 C5 C8 121.2(3) . .
C5 C6 H6 120.1 . .
C7 C6 C5 119.9(3) . .
C7 C6 H6 120.1 . .
N2 C7 C6 122.8(3) . .
N2 C7 H7 118.6 . .
C6 C7 H7 118.6 . .
C5 C8 H8A 108.3 . .
C5 C8 H8B 108.3 . .
H8A C8 H8B 107.4 . .
N9 C8 C5 115.7(3) . .
N9 C8 H8A 108.3 . .
N9 C8 H8B 108.3 . .
C8 N9 Ag1 105.55(18) . .
C10 N9 Ag1 108.7(2) . .
C10 N9 C8 112.1(2) . .
C14 N9 Ag1 109.96(19) . .
C14 N9 C8 111.8(3) . .
C14 N9 C10 108.7(2) . .
N9 C10 H10A 109.7 . .
N9 C10 H10B 109.7 . .
N9 C10 C11 109.8(3) . .
H10A C10 H10B 108.2 . .
C11 C10 H10A 109.7 . .
C11 C10 H10B 109.7 . .
C10 C11 H11A 109.6 . .
C10 C11 H11B 109.6 . .
H11A C11 H11B 108.1 . .
N12 C11 C10 110.1(3) . .
N12 C11 H11A 109.6 . .
N12 C11 H11B 109.6 . .
C13 N12 C11 110.6(3) . .
C15 N12 C11 111.7(3) . .
C15 N12 C13 110.5(3) . .
N12 C13 H13A 109.4 . .
N12 C13 H13B 109.4 . .
N12 C13 C14 111.0(3) . .
H13A C13 H13B 108.0 . .
C14 C13 H13A 109.4 . .
C14 C13 H13B 109.4 . .
N9 C14 C13 110.4(3) . .
N9 C14 H14A 109.6 . .
N9 C14 H14B 109.6 . .
C13 C14 H14A 109.6 . .
C13 C14 H14B 109.6 . .
H14A C14 H14B 108.1 . .
N12 C15 H15A 108.9 . .
N12 C15 H15B 108.9 . .
N12 C15 C16 113.3(3) . .
H15A C15 H15B 107.7 . .
C16 C15 H15A 108.9 . .
C16 C15 H15B 108.9 . .
C17 C16 C15 122.0(3) . .
C17 C16 C18 117.7(3) . .
C18 C16 C15 120.2(3) . .
C16 C17 H17 119.6 . .
C18 C17 C16 120.8(3) 2_585 .
C18 C17 H17 119.6 2_585 .
C16 C18 H18 119.3 . .
C17 C18 C16 121.5(3) 2_585 .
C17 C18 H18 119.3 2_585 .
S20 O19 Ag1 153.4(2) . .
O19 S20 O21 113.0(2) . .
O19 S20 C23 103.7(2) . .
O21 S20 C23 102.7(2) . .
O22 S20 O19 115.03(19) . .
O22 S20 O21 115.61(19) . .
O22 S20 C23 104.8(2) . .
S20 O21 Ag1 100.64(15) . 2_666
F24 C23 S20 110.6(3) . .
F25 C23 S20 110.5(3) . .
F25 C23 F24 107.7(4) . .
F26 C23 S20 111.6(3) . .
F26 C23 F24 109.0(4) . .
F26 C23 F25 107.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N2 2.161(3) 1_655
Ag1 N9 2.243(3) .
Ag1 O19 2.591(3) .
Ag1 O21 2.828(3) 2_666
N2 Ag1 2.161(3) 1_455
N2 C3 1.344(4) .
N2 C7 1.348(5) .
C3 H3 0.9500 .
C3 C4 1.382(5) .
C4 H4 0.9500 .
C4 C5 1.394(5) .
C5 C6 1.398(5) .
C5 C8 1.508(4) .
C6 H6 0.9500 .
C6 C7 1.374(5) .
C7 H7 0.9500 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C8 N9 1.497(4) .
N9 C10 1.475(4) .
N9 C14 1.467(4) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C10 C11 1.511(4) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C11 N12 1.467(4) .
N12 C13 1.461(4) .
N12 C15 1.459(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C13 C14 1.516(4) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C15 C16 1.512(5) .
C16 C17 1.388(5) .
C16 C18 1.401(5) .
C17 H17 0.9500 .
C17 C18 1.384(5) 2_585
C18 C17 1.384(5) 2_585
C18 H18 0.9500 .
O19 S20 1.434(3) .
S20 O21 1.438(3) .
S20 O22 1.428(3) .
S20 C23 1.822(5) .
O21 Ag1 2.828(3) 2_666
C23 F24 1.337(6) .
C23 F25 1.331(5) .
C23 F26 1.325(6) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Ag1 N2 C3 C4 178.7(2) 1_455 .
Ag1 N2 C7 C6 -179.7(3) 1_455 .
Ag1 N9 C10 C11 58.9(3) . .
Ag1 N9 C14 C13 -59.7(3) . .
Ag1 O19 S20 O21 148.7(5) . .
Ag1 O19 S20 O22 13.0(6) . .
Ag1 O19 S20 C23 -100.9(5) . .
N2 C3 C4 C5 1.2(5) . .
C3 N2 C7 C6 0.2(5) . .
C3 C4 C5 C6 -0.1(5) . .
C3 C4 C5 C8 177.5(3) . .
C4 C5 C6 C7 -0.8(5) . .
C4 C5 C8 N9 97.3(4) . .
C5 C6 C7 N2 0.8(5) . .
C5 C8 N9 Ag1 -179.0(2) . .
C5 C8 N9 C10 62.8(4) . .
C5 C8 N9 C14 -59.5(4) . .
C6 C5 C8 N9 -85.2(4) . .
C7 N2 C3 C4 -1.2(5) . .
C8 C5 C6 C7 -178.4(3) . .
C8 N9 C10 C11 175.2(3) . .
C8 N9 C14 C13 -176.6(3) . .
N9 C10 C11 N12 60.1(4) . .
C10 N9 C14 C13 59.2(3) . .
C10 C11 N12 C13 -57.2(4) . .
C10 C11 N12 C15 179.3(3) . .
C11 N12 C13 C14 55.7(4) . .
C11 N12 C15 C16 -66.5(4) . .
N12 C13 C14 N9 -57.2(4) . .
N12 C15 C16 C17 -32.2(5) . .
N12 C15 C16 C18 151.1(3) . .
C13 N12 C15 C16 170.0(3) . .
C14 N9 C10 C11 -60.8(3) . .
C15 N12 C13 C14 180.0(3) . .
C15 C16 C17 C18 -176.1(3) . 2_585
C15 C16 C18 C17 176.1(3) . 2_585
C17 C16 C18 C17 -0.7(5) . 2_585
C18 C16 C17 C18 0.7(5) . 2_585
O19 S20 O21 Ag1 -23.1(2) . 2_666
O19 S20 C23 F24 -53.6(4) . .
O19 S20 C23 F25 65.6(4) . .
O19 S20 C23 F26 -175.1(3) . .
O21 S20 C23 F24 64.3(4) . .
O21 S20 C23 F25 -176.6(4) . .
O21 S20 C23 F26 -57.2(4) . .
O22 S20 O21 Ag1 112.43(19) . 2_666
O22 S20 C23 F24 -174.6(3) . .
O22 S20 C23 F25 -55.4(4) . .
O22 S20 C23 F26 64.0(4) . .
C23 S20 O21 Ag1 -134.08(19) . 2_666
