Energetic transition metal complexes based on methyl carbazate and picric acid: syntheses, structures, physicochemical properties and catalysis on the thermal decomposition of ammonium perchlorate
Yang, Xiaoming; Wang, Yanna; Li, Zhimin; Du, Jiang; Wang, Lin; Zhang, Tonglai; New Journal of Chemistry 43 (2019) 14159–; doi:10.1039/C9NJ03591E

data_7058740
_publ_section_title
;
 Energetic transition metal complexes based on methyl carbazate and picric
 acid: syntheses, structures, physicochemical properties and catalysis on
 the thermal decomposition of ammonium perchlorate
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14159
_journal_paper_doi               10.1039/C9NJ03591E
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C4 H18 Cd N4 O7, 2(C6 H2 N3 O7), 4(H2 O)'
_chemical_formula_sum            'C16 H30 Cd N10 O25'
_chemical_formula_weight         874.90
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-27 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.02(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.551(3)
_cell_length_b                   8.5075(17)
_cell_length_c                   30.293(6)
_cell_measurement_reflns_used    4864
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      0.6806
_cell_volume                     3194.6(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            12527
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         2.723
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0255P)^2^+11.4418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3430
_reflns_number_total             3619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03591e2.cif
_cod_data_source_block           bwn18209_pl
_cod_depositor_comments
'Adding full bibliography for 7058734--7058740.cif.'
_cod_database_code               7058740
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.903
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups, All O(H) groups, All
  O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 O11(H11A,H11B), O12(H12), N1(H1), N2(H2A,H2B), O10(H10A,H10B), O13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8)
2.c Idealised Me refined as rotating group:
 C2(H2C,H2D,H2E)
;
_olex2_submission_special_instructions 'No special instructions were received'