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_7712044
_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         '2(C4 H5 Cd0.5 N8)'
_chemical_formula_sum            'C8 H10 Cd N16'
_chemical_formula_weight         442.72
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-19
_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                93.655(7)
_cell_angle_beta                 93.742(6)
_cell_angle_gamma                110.729(9)
_cell_formula_units_Z            2
_cell_length_a                   7.5280(6)
_cell_length_b                   8.7978(11)
_cell_length_c                   13.4483(9)
_cell_measurement_reflns_used    5402
_cell_measurement_temperature    298.21(10)
_cell_measurement_theta_max      28.4830
_cell_measurement_theta_min      2.4710
_cell_volume                     827.64(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_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      298.21(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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    -62.00  42.00   0.50    0.05    --   10.52 -77.00-120.00  208
  2  \w     24.00  57.00   0.50    0.05    --   10.52-138.00-116.00   66
  3  \w     23.00  50.00   0.50    0.05    --   10.52-131.00  59.00   54
  4  \w    -28.00  51.00   0.50    0.05    --  -11.30  19.00-180.00  158
  5  \w    -25.00  25.00   0.50    0.05    --  -11.30  19.00 -30.00  100
  6  \w     35.00  60.00   0.50    0.05    --  -11.30  19.00 -30.00   50
  7  \w    -44.00  57.00   0.50    0.05    --  -11.30  77.00  30.00  202
  8  \w    -72.00 -47.00   0.50    0.05    --  -11.30 138.00 -54.00   50
  9  \w    -74.00 -49.00   0.50    0.05    --  -11.30 131.00 130.00   50
 10  \w    -10.00  34.00   0.50    0.05    --  -11.30 -99.00-150.00   88
;
_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      -0.0226081000
_diffrn_orient_matrix_UB_12      0.0709305000
_diffrn_orient_matrix_UB_13      -0.0054541000
_diffrn_orient_matrix_UB_21      0.0089313000
_diffrn_orient_matrix_UB_22      0.0162317000
_diffrn_orient_matrix_UB_23      0.0527954000
_diffrn_orient_matrix_UB_31      0.0982290000
_diffrn_orient_matrix_UB_32      0.0469205000
_diffrn_orient_matrix_UB_33      -0.0009073000
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10419
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.388
_diffrn_reflns_theta_min         1.524
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.64a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       slice
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0300(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0343P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2855
_reflns_number_total             3676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03180a2.cif
_cod_data_source_block           xhh-248131
_cod_depositor_comments
'Adding full bibliography for 7712042--7712045.cif.'
_cod_database_code               7712044
_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.a Rotating group:
 N15(H15a,H15b), N25(H25a,H25b)
2.b Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C11(H11a,H11b,H11c)
;
_shelx_res_checksum              80541
_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 1.584
_oxdiff_exptl_absorpt_empirical_full_min 0.636