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_7245063
_publ_section_title
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 Topological motifs in dicyanamides of transition metals
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00485B
_journal_year                    2022
_chemical_formula_moiety         '0.17(C120 H96 Cu6 N60)'
_chemical_formula_sum            'C20 H16 Cu N10'
_chemical_formula_weight         459.97
_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   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                96.162(2)
_cell_angle_beta                 103.516(2)
_cell_angle_gamma                99.484(2)
_cell_formula_units_Z            6
_cell_length_a                   12.2316(6)
_cell_length_b                   13.1085(7)
_cell_length_c                   18.7874(10)
_cell_measurement_reflns_used    4369
_cell_measurement_temperature    170
_cell_measurement_theta_max      24.599
_cell_measurement_theta_min      3.017
_cell_volume                     2855.3(3)
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.994
_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  0.0497
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            276637
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.066
_diffrn_reflns_theta_min         2.256
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       prism
_exptl_crystal_F_000             1410
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         19837
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+30.7526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6463
_reflns_number_total             19837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00485b3.cif
_cod_data_source_block           merabet_ma505_0m_a
_cod_database_code               7245063
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.726
_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
Uanis(C15) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 N20(H20), N22(H22), N24(H24), N26(H26), N28(H28), N30(H30), C17(H17),
 C18(H18), C19(H19), C20(H20A), C25(H25), C26(H26A), C27(H27), C28(H28A),
 C33(H33), C34(H34), C35(H35), C36(H36), C41(H41), C42(H42), C43(H43), C44(H44),
  C49(H49), C50(H50), C51(H51), C52(H52), C57(H57), C58(H58), C59(H59), C60(H60)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C38(H38A,H38B,
 H38C), C46(H46A,H46B,H46C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              12353
_olex2_submission_special_instructions 'No special instructions were received'