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_7240109
_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         'C14 H20 Br6 N4 Zn2, 2(H2 O)'
_chemical_formula_sum            'C14 H24 Br6 N4 O2 Zn2'
_chemical_formula_weight         890.57
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-23 deposited with the CCDC.	2020-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                99.830(18)
_cell_angle_beta                 95.106(18)
_cell_angle_gamma                103.695(19)
_cell_formula_units_Z            1
_cell_length_a                   7.458(5)
_cell_length_b                   9.586(6)
_cell_length_c                   9.603(6)
_cell_measurement_reflns_used    3317
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.409
_cell_measurement_theta_min      3.127
_cell_volume                     651.2(7)
_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      298
_diffrn_measured_fraction_theta_full 0.861
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.861
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3741
_diffrn_reflns_point_group_measured_fraction_full 0.861
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         25.488
_diffrn_reflns_theta_min         2.231
_exptl_absorpt_coefficient_mu    11.063
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1633 before and 0.0707 after correction. The Ratio of minimum to maximum transmission is 0.3471. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_description       plate
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.916
_refine_diff_density_rms         0.538
_refine_ls_extinction_coef       0.173(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2087
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0966
_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^)+(0.1417P)^2^+3.7471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2295
_refine_ls_wR_factor_ref         0.2491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1748
_reflns_number_total             2087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00093k2.cif
_cod_data_source_block           20180713_1a_0m
_cod_database_code               7240109
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.511
_shelx_estimated_absorpt_t_min   0.404
_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 O(H,H) groups
2. Restrained distances
 H1A-H1E
 2.2 with sigma of 0.02
3.a Free rotating group:
 O1(H1E,H1F)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), N1(H1A,H1B), C1(H1C,H1D)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C4(H4)
;
_shelx_res_checksum              71109
_olex2_submission_special_instructions 'No special instructions were received'