Synthesis, decomposition studies and crystal structure of a three-dimensional CuCN network structure with protonated <i>N</i>-methylethanolamine as the guest cation
Koenigsmann, Christopher; Rachid, Leena N.; Sheedy, Christina M.; Corfield, Peter W. R.; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620004477

data_2022083
_publ_section_title
;
 Synthesis, decomposition studies and crystal structure of a
 three-dimensional CuCN network structure with protonated
 <i>N</i>-methylethanolamine as the guest cation
;
_journal_coeditor_code           OP3005
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620004477
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '(C3 H10 N O) [Cu2 (C N)3]'
_chemical_formula_moiety         'C3 H10 N O +, C3 N3 Cu2 -'
_chemical_formula_sum            'C6 H10 Cu2 N4 O'
_chemical_formula_weight         281.26
_chemical_name_systematic
'Poly[2-hydroxy-<i>N</i>-methylethan-1-aminium [\m~3~-cyanido-\k^3^<i>C</i>:<i>C</i>:<i>N</i>-di-\m-cyanido-\k^4^<i>C</i>:<i>N</i>-dicuprate(I)]]'
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8994(5)
_cell_length_b                   8.8994(5)
_cell_length_c                   11.3750(11)
_cell_measurement_reflns_used    2071
_cell_measurement_temperature    303.0(10)
_cell_measurement_theta_max      34.97
_cell_measurement_theta_min      1.00
_cell_volume                     900.89(11)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
KappaCCD Server Software (Nonius, 1997)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 (Farrugia, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      303.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Enraf--Nonius KappaCCD'
_diffrn_measurement_method       'combination of \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3962
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         34.956
_diffrn_reflns_theta_min         2.288
_exptl_absorpt_coefficient_mu    4.683
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.412
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1606 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.008(8)
_refine_ls_extinction_coef       0.0066(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2017 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0090P)^2^+0.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0483
_reflns_number_gt                3685
_reflns_number_total             3962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            op3005sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        900.89(13)
_cod_database_code               2022083
_shelx_estimated_absorpt_t_min   0.334
_shelx_estimated_absorpt_t_max   0.735
_shelx_hkl_checksum              50838
_shelx_res_checksum              60989
_cod_database_fobs_code 2022083