Liquid reagents are not enough for liquid assisted grinding in the synthesis of [(AgBr)(<i>n</i>-pica)]<sub><i>n</i></sub>.
Zuffa, Caterina; Cappuccino, Chiara; Casali, Lucia; Emmerling, Franziska; Maini, Lucia; Physical chemistry chemical physics : PCCP 26 (2024) 5010–5019; doi:10.1039/d3cp04791a

data_7247950
_publ_section_title
;
 Liquid reagents are not enough for liquid assisted grinding in the
 synthesis of [(AgBr)(<i>n</i>-pica)]<sub><i>n</i></sub>.
;
_journal_issue                   6
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              5010
_journal_page_last               5019
_journal_paper_doi               10.1039/d3cp04791a
_journal_volume                  26
_journal_year                    2024
_chemical_compound_source        'solvothermal synthesis'
_chemical_formula_moiety         'C6 H8 Ag2 Br2 N2'
_chemical_formula_sum            'C6 H8 Ag2 Br2 N2'
_chemical_formula_weight         483.68
_chemical_melting_point          379
_chemical_name_systematic        '[(AgBr)2(3-pica)]n'
_chemical_properties_physical    Light-sensitive
_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     dual
_audit_creation_date             2022-07-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-10-02 deposited with the CCDC.	2024-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.938(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.605(3)
_cell_length_b                   6.2851(5)
_cell_length_c                   14.3050(12)
_cell_measurement_reflns_used    844
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5590
_cell_measurement_theta_min      4.0300
_cell_volume                     2066.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -78.00 -47.00   1.00  125.00    --  -16.36 -77.00 -30.00   31
  2  \w    -24.00  24.00   1.00  125.00    --  -16.36 -99.00-120.00   48
  3  \w    -84.00  -4.00   1.00  125.00    --  -16.36 -57.00  90.00   80
  4  \w     38.00  92.00   1.00  125.00    --   17.61-178.00 -60.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0294315000
_diffrn_orient_matrix_UB_12      0.0299935000
_diffrn_orient_matrix_UB_13      0.0190226000
_diffrn_orient_matrix_UB_21      0.0376815000
_diffrn_orient_matrix_UB_22      0.0646579000
_diffrn_orient_matrix_UB_23      0.0159743000
_diffrn_orient_matrix_UB_31      -0.0177319000
_diffrn_orient_matrix_UB_32      0.0875812000
_diffrn_orient_matrix_UB_33      -0.0182871000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.1454
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4378
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.984
_diffrn_reflns_theta_min         3.360
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.474
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.110
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1742
_refine_ls_R_factor_gt           0.0726
_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/[\s^2^(Fo^2^)+(0.0259P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1170
_reflns_number_total             2359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp04791a2.cif
_cod_data_source_block           AgBr2_3pica_final
_cod_depositor_comments
'Adding full bibliography for 7247949--7247950.cif.'
_cod_original_cell_volume        2066.2(3)
_cod_database_code               7247950
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C6(H6), C2(H2)
;
_shelx_res_checksum              71366
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.229
_oxdiff_exptl_absorpt_empirical_full_min 0.360