Effect of stepwise protonation of an N-containing ligand on the formation of metal-organic salts and coordination complexes in the solid state
Lu, Hai Dong; Li, Hai Tao; Xin, Lianxin; Guo, Fang; CrystEngComm  (2020) –; doi:10.1039/D0CE00093K

data_7240114
_publ_section_title
;
 Effect of stepwise protonation of an N-containing ligand on the formation
 of metal-organic salts and coordination complexes in the solid state
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00093K
_journal_year                    2020
_chemical_formula_moiety         '2(Br4 Cu), C14 H22 N4'
_chemical_formula_sum            'C14 H22 Br8 Cu2 N4'
_chemical_formula_weight         1012.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-12 deposited with the CCDC.	2020-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.842(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7157(13)
_cell_length_b                   22.709(4)
_cell_length_c                   7.5681(13)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.388
_cell_measurement_theta_min      3.192
_cell_volume                     1325.9(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20406
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         28.434
_diffrn_reflns_theta_min         3.193
_exptl_absorpt_coefficient_mu    13.668
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1757 before and 0.0856 after correction.
The Ratio of minimum to maximum transmission is 0.3125.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.087
_refine_diff_density_min         -1.784
_refine_diff_density_rms         0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         3321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0606P)^2^+14.8758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2949
_reflns_number_total             3321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00093k2.cif
_cod_data_source_block           20180710_4a_0m
_cod_database_code               7240114
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.408
_shelx_estimated_absorpt_t_min   0.145
_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
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C2(H2A,H2B), C1(H1C,H1D)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C6(H6), C5(H5)
;
_shelx_res_checksum              91621
_olex2_submission_special_instructions 'No special instructions were received'