Crystal structure of [2,13-bis(acetamido)-5,16-dimethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane-κ^4^<i>N</i>]silver(II) dinitrate from synchrotron X-ray data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 74 (2018) 461–464; doi:10.1107/S2056989018003560

data_2243631
_publ_section_title
;
 Crystal structure of
 [2,13-bis(acetamido)-5,16-dimethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane-\k^4^<i>N</i>]silver(II)
 dinitrate from synchrotron X-ray data
;
_journal_coeditor_code           SJ5548
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              461
_journal_page_last               464
_journal_paper_doi               10.1107/S2056989018003560
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Ag (C24 H46 N6 O2)] (N O3)2'
_chemical_formula_moiety         'C24 H46 Ag N6 O2 2+, 2(N O3 -)'
_chemical_formula_sum            'C24 H46 Ag N8 O8'
_chemical_formula_weight         682.56
_chemical_name_systematic
'[(5,16-Dimethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane-2,13-diyl)diacetamide-\k^4^<i>N</i>^2^,<i>N</i>^6^,<i>N</i>^13^,<i>N</i>^17^]silver(II) dinitrate'
_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
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                104.32(3)
_cell_angle_beta                 90.28(3)
_cell_angle_gamma                109.60(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3460(17)
_cell_length_b                   9.2874(19)
_cell_length_c                   10.171(2)
_cell_measurement_reflns_used    46429
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.350
_cell_volume                     716.3(3)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL BL2D-SMDC Program</i> (Shin <i>et al.,</i> 2016)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
<i>DIAMOND 4</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.610
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            7431
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.782
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             357
_exptl_crystal_size_max          0.021
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.713
_refine_diff_density_min         -2.172
_refine_ls_extinction_coef       0.065(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0747P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                3418
_reflns_number_total             3750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5548sup1.cif
_cod_data_source_block           I
_cod_database_code               2243631
_shelx_estimated_absorpt_t_min   0.989
_shelx_estimated_absorpt_t_max   0.993
_shelx_hkl_checksum              87107
_shelx_res_checksum              6241
_cod_database_fobs_code 2243631