Topological motifs in dicyanamides of transition metals
Merabet, Layachi; Vologzhanina, Anna V.; Setifi, Zouaoui; Kaboub, Lakhmissi; Setifi, Fatima; CrystEngComm  (2022) –; doi:10.1039/D2CE00485B

data_7245059
_publ_section_title
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 Topological motifs in dicyanamides of transition metals
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00485B
_journal_year                    2022
_chemical_formula_moiety         'C12 H7 Fe N11, 0.5(C2 H3 N)'
_chemical_formula_sum            'C13 H8.5 Fe N11.5'
_chemical_formula_weight         381.66
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-01 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.0011(7)
_cell_length_b                   15.7369(5)
_cell_length_c                   8.9768(3)
_cell_measurement_reflns_used    1387
_cell_measurement_temperature    170
_cell_measurement_theta_max      24.39
_cell_measurement_theta_min      2.97
_cell_volume                     3523.85(19)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex 2 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1791
_diffrn_reflns_av_unetI/netI     0.2620
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            84629
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.519
_diffrn_reflns_theta_min         2.589
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       plate
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         5374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0552P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2767
_reflns_number_total             5374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00485b3.cif
_cod_data_source_block           sz120
_cod_original_formula_sum        'C13 H8.50 Fe N11.50'
_cod_database_code               7245059
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.704
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(N7A) = Uiso(N7)
3. Others
 Fixed Sof: N7(0.5) N10(0.5) N7A(0.5) N10A(0.5) C1S(0.5) N1S(0.5) C2S(0.5)
 H2SA(0.5) H2SB(0.5) H2SC(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C3(H3A), C6(H6), C7(H7), C8(H8)
4.b Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              25096
_olex2_submission_special_instructions 'No special instructions were received'