Coordination polymerization of nitrogen-rich linkers and dicyanamide anions toward energetic coordination polymers with low sensitivities.
Xie, Hao-Hui; Wang, Qin; Weng, Jiao-Lin; Yan, Yun-Fan; Bian, Hong-Yi; Huang, Ying; Zheng, Fa-Kun; Qiu, Ren-Hui; Xu, Jian-Gang; Dalton transactions (Cambridge, England : 2003) 52 (2023) 818–824; doi:10.1039/d2dt03180a

data_7712045
_publ_section_title
;
 Coordination polymerization of nitrogen-rich linkers and dicyanamide
 anions toward energetic coordination polymers with low sensitivities.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              818
_journal_page_last               824
_journal_paper_doi               10.1039/d2dt03180a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C6 H5 Cu N11'
_chemical_formula_sum            'C6 H5 Cu N11'
_chemical_formula_weight         294.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-29
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-10-31 deposited with the CCDC.	2022-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.854(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5555(6)
_cell_length_b                   7.8169(3)
_cell_length_c                   11.9927(5)
_cell_measurement_reflns_used    4305
_cell_measurement_temperature    296.76(10)
_cell_measurement_theta_max      27.1830
_cell_measurement_theta_min      1.7570
_cell_volume                     1080.83(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.76(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.805
_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    -10.00  25.00   0.50    0.63    --  -11.30 -99.00 -60.00   70
  2  \w    -11.00  14.00   0.50    0.63    --  -11.30 -99.00  30.00   50
  3  \w    -10.00  55.00   0.50    0.63    --   10.52 -99.00  90.00  130
  4  \w    -41.00  47.00   0.50    0.63    --   10.52 -82.00 171.00  176
  5  \w     15.00  82.00   0.50    0.63    --   10.52  57.00 -90.00  134
  6  \w     -2.00  36.00   0.50    0.63    --  -11.30  82.00 -66.00   76
  7  \w    -35.00  -9.00   0.50    0.63    --  -11.30  82.00 -66.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0419190000
_diffrn_orient_matrix_UB_12      0.0461717000
_diffrn_orient_matrix_UB_13      0.0284625000
_diffrn_orient_matrix_UB_21      0.0420245000
_diffrn_orient_matrix_UB_22      0.0636188000
_diffrn_orient_matrix_UB_23      0.0148763000
_diffrn_orient_matrix_UB_31      -0.0162542000
_diffrn_orient_matrix_UB_32      0.0453628000
_diffrn_orient_matrix_UB_33      -0.0497811000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8589
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.355
_diffrn_reflns_theta_min         1.766
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.024
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_description       needle
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0505P)^2^+0.1891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1850
_reflns_number_total             2394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03180a2.cif
_cod_data_source_block           xhh-129131_autored
_cod_depositor_comments
'Adding full bibliography for 7712042--7712045.cif.'
_cod_database_code               7712045
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed X: Cu1(0.16148)
 Fixed Y: Cu1(0.39067)
 Fixed Z: N15(0.38495)
3.a X=CH2 refined with riding coordinates:
 N25(H25a,H25b)
3.b Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c)
;
_shelx_res_checksum              68542
_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 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.798