Coordination Chemistry and Structural Dynamics of a Long and Flexible Piperazine-Derived Ligand.
Hawes, Chris S.; Hamilton, Sophie E.; Hicks, Jamie; Knowles, Gregory P.; Chaffee, Alan L.; Turner, David R.; Batten, Stuart R.; Inorganic chemistry 55 (2016) 6692–6702; doi:10.1021/acs.inorgchem.6b00933

data_4348068
_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         '0.25(C112 H144 Ag8 N24), C4 H6 N2, 2(B F4)'
_chemical_formula_sum            'C32 H42 Ag2 B2 F8 N8'
_chemical_formula_weight         928.09
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 91.87(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.282(3)
_cell_length_b                   22.790(5)
_cell_length_c                   13.580(3)
_cell_measurement_reflns_used    17743
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.323
_cell_measurement_theta_min      1.885
_cell_volume                     3799.1(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24004
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         1.885
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.950
_refine_diff_density_min         -1.782
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4699
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+18.5720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1349
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4040
_reflns_number_total             4699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00933_si_002.cif
_cod_data_source_block           4
_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_original_cell_volume        3799.2(15)
_cod_database_code               4348068
_olex2_refinement_description
;
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
2. Restrained distances
 C29-N28
 1.15 with sigma of 0.02
 C26-C26_$1
 1.75 with sigma of 0.02
 C26-N25
 1.15 with sigma of 0.02
 C29-C30
 1.5 with sigma of 0.02
 C27-C26
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(N25) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C26(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) N28(0.5) C29(0.5)
 C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C18(H18), C19(H19)
5.c Idealised Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              50571
_shelx_hkl_checksum              79720
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'