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_7712042
_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         'C8 H10 Co N16, H2 O'
_chemical_formula_sum            'C8 H12 Co N16 O'
_chemical_formula_weight         407.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-20
_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                 102.687(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3406(4)
_cell_length_b                   15.4425(7)
_cell_length_c                   14.6670(9)
_cell_measurement_reflns_used    6849
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      28.8880
_cell_measurement_theta_min      1.9330
_cell_volume                     1622.02(16)
_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      N~2~
_diffrn_ambient_temperature      99.99(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 0.804
_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      0.00  30.00   0.50    0.61    --  -11.30 -99.00-150.00   60
  2  \w    -11.00  14.00   0.50    0.61    --  -11.30 -99.00-180.00   50
  3  \w     -8.00  22.00   0.50    0.61    --  -11.30 -99.00-120.00   60
  4  \w     -6.00  29.00   0.50    0.61    --  -11.30 -99.00  30.00   70
  5  \w    -59.00  34.00   0.50    0.61    --   10.52 -58.00   3.00  186
  6  \w     19.00  84.00   0.50    0.61    --   10.52  58.00 144.00  130
;
_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      0.0416696000
_diffrn_orient_matrix_UB_12      -0.0085063000
_diffrn_orient_matrix_UB_13      0.0473744000
_diffrn_orient_matrix_UB_21      0.0610120000
_diffrn_orient_matrix_UB_22      -0.0303550000
_diffrn_orient_matrix_UB_23      -0.0141939000
_diffrn_orient_matrix_UB_31      0.0659997000
_diffrn_orient_matrix_UB_32      0.0334540000
_diffrn_orient_matrix_UB_33      -0.0008635000
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10729
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.245
_diffrn_reflns_theta_min         1.940
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49600
_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            red
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       needle
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3544
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0472P)^2^+1.7697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3095
_reflns_number_total             3544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03180a2.cif
_cod_data_source_block           xhh-21203
_cod_depositor_comments
'Adding full bibliography for 7712042--7712045.cif.'
_cod_database_code               7712042
_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. Restrained distances
 H22A-H22B \\sim H22B-H22C
 with sigma of 0.02
 H24A-H24B \\sim H24B-H24C
 with sigma of 0.02
3.a X=CH2 refined with riding coordinates:
 N30(H30A,H30B), N25(H25A,H25B)
3.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              77514
_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 1.460
_oxdiff_exptl_absorpt_empirical_full_min 0.361