Templating Effect of Trans-2,5-dimethylpiperazine (TDMP) on the Structure Dimensionality of Hybrid Metal Halides
Gautier, Romain; PARIS, Michael; Massuyeau, Florian; Dalton Transactions  (2022) –; doi:10.1039/D2DT00614F

data_7710160
_publ_section_title
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 Templating Effect of Trans-2,5-dimethylpiperazine (TDMP) on the Structure
 Dimensionality of Hybrid Metal Halides
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00614F
_journal_year                    2022
_chemical_formula_moiety         '2(C3 H8 N), Br4 Cu'
_chemical_formula_sum            'C6 H16 Br4 Cu N2'
_chemical_formula_weight         499.367
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2022-04-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-26 deposited with the CCDC.	2022-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                92.2638(15)
_cell_angle_beta                 97.7120(17)
_cell_angle_gamma                90.2231(16)
_cell_formula_units_Z            2
_cell_length_a                   7.20781(14)
_cell_length_b                   7.23746(13)
_cell_length_c                   13.4221(2)
_cell_measurement_reflns_used    85
_cell_measurement_temperature    293
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     693.28(2)
_computing_data_collection       Supergui
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004  (Burla et al.,  2007)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9830
_diffrn_measured_fraction_theta_max 0.9865
_diffrn_measurement_device_type  'Bruker-Nonius Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.9830
_diffrn_reflns_Laue_measured_fraction_max 0.9865
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22934
_diffrn_reflns_point_group_measured_fraction_full 0.9830
_diffrn_reflns_point_group_measured_fraction_max 0.9865
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         6.42
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    13.067
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1379 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.6162.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.392
_exptl_crystal_description       block
_exptl_crystal_F_000             469.292
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.7225
_refine_diff_density_min         -0.7643
_refine_diff_density_rms         0.1474
_refine_ls_d_res_high            0.7545
_refine_ls_d_res_low             3.1804
_refine_ls_extinction_coef       0.0026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0597
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     121
_refine_ls_number_reflns         3354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0597
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0073P)^2^+0.6757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0373
_refine_ls_wR_factor_ref         0.0416
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              9
_reflns_limit_k_min              -9
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                2735
_reflns_number_total             3354
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt00614f1.cif
_cod_data_source_block           shelx
_cod_database_code               7710160
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 N2(H2a,H2b), N3(H3a,H3b), C3(H3c,H3d), C4(H4a,H4b)
2.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c)
;
_olex2_submission_special_instructions 'No special instructions were received'