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_4348070
_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), 0.5(C4 H8 O2), 2(B F4)'
_chemical_formula_sum            'C30 H40 Ag2 B2 F8 N6 O'
_chemical_formula_weight         890.04
_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
_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                 91.819(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.975(8)
_cell_length_b                   23.050(2)
_cell_length_c                   13.155(3)
_cell_measurement_reflns_used    10462
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.969
_cell_measurement_theta_min      1.802
_cell_volume                     3932(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 0.995
_diffrn_measured_fraction_theta_max 0.991
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18646
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.969
_diffrn_reflns_theta_min         1.802
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.849
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4693
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0881P)^2^+14.3002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3410
_reflns_number_total             4693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00933_si_002.cif
_cod_data_source_block           6
_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               4348070
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 B26-F31
 1.45 with sigma of 0.02
 F30-B26
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F30) \\sim Ueq, Uanis(F31) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: O20(0.25) C21(0.25) H21A(0.25) H21B(0.25) C22(0.25) H22A(0.25)
 H22B(0.25) O23(0.25) C24(0.25) H24A(0.25) H24B(0.25) C25(0.25) H25B(0.25)
 H25A(0.25) F30(0.5) F31(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), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C25(H25B,H25A)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C18(H18), C19(H19)
;
_shelx_res_checksum              86109
_shelx_hkl_checksum              41437
_shelx_fab_checksum              10342
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'