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_7240113
_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         '4(I), C14 H22 N4, 2(C H4 O)'
_chemical_formula_sum            'C16 H30 I4 N4 O2'
_chemical_formula_weight         818.04
_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   geom
_audit_creation_date             2019-04-25
_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                 93.907(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0705(6)
_cell_length_b                   20.8072(16)
_cell_length_c                   7.8346(6)
_cell_measurement_reflns_used    9148
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.308
_cell_measurement_theta_min      3.260
_cell_volume                     1312.56(17)
_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)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16112
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.260
_exptl_absorpt_coefficient_mu    4.764
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1292 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.3493.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.070
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0140P)^2^+9.2472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2201
_reflns_number_total             2253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00093k2.cif
_cod_data_source_block           20190411_1a_0m
_cod_database_code               7240113
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.449
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(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:
 N2(H2), C7(H7), C4(H4), C6(H6), C5(H5)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              9167
_olex2_submission_special_instructions 'No special instructions were received'