Solvatochromism as a probe to observe the solvent exchange process in a 1-D porous coordination polymer with 1-D solvent accessible channels.
Barbour, Len; Bezuidenhout, Charl Xavier; Esterhuysen, Catharine; Chem. Commun.  (2017) –; doi:10.1039/C7CC02492D

data_7120047
_publ_section_title
;
 Solvatochromism as a probe to observe the solvent exchange process in a
 1-D porous coordination polymer with 1-D solvent accessible channels.
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02492D
_journal_year                    2017
_chemical_formula_moiety         '0.13(C20 H20 Cu2 N6 O8), 0.25(C H3 N O2)'
_chemical_formula_sum            'C2.75 H3.25 Cu0.25 N O1.5'
_chemical_formula_weight         90.20
_chemical_name_systematic        Cu(OAc)2Dptz.(Nitromethane)
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-03-31 deposited with the CCDC.
2017-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                92.401(3)
_cell_angle_beta                 101.341(3)
_cell_angle_gamma                97.641(2)
_cell_formula_units_Z            8
_cell_length_a                   7.2601(15)
_cell_length_b                   8.0089(17)
_cell_length_c                   12.696(3)
_cell_measurement_reflns_used    4572
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      2.57
_cell_volume                     715.6(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7802
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.64
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.562
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1479 before and 0.0287 after correction.
The Ratio of minimum to maximum transmission is 0.8034.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_recrystallization_method 'solvent exchange'
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3294
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.4348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                3051
_reflns_number_total             3294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc02492d11.cif
_cod_data_source_block           solve2
_cod_original_formula_sum        'C2.75 H3.25 Cu0.25 N O1.50'
_cod_database_code               7120047
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C31-C41A \\sim C31-C21A \\sim C31-C21B \\sim C31-C41B
 with sigma of 0.02
 N11-C11A \\sim N11-C51A \\sim N11-C51B \\sim N11-C11B
 with sigma of 0.02
 C61-N31A \\sim C61-N21B \\sim C61-N31B \\sim C61-N21A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21B) = Uanis(C21A) = Uanis(C41A) = Uanis(C41B) = Uanis(C51A) =
Uanis(C51B) = Uanis(C11B) = Uanis(C11A) = Uanis(N31B)
Uvol(N31B) \\sim Uvol(N31A) \\sim Uvol(N21A) \\sim Uvol(N21B): with sigma of 0.1
4. Others
 Fixed Sof: N31A(0.63011) N21A(0.63011) C11A(0.63011) H11A(0.63011)
 C21A(0.63011) H21A(0.63011) C41A(0.63011) H41A(0.63011) C51A(0.63011)
 H51A(0.63011) N31B(0.36989) N21B(0.36989) C11B(0.36989) H11B(0.36989)
 C21B(0.36989) H21B(0.36989) C41B(0.36989) H41B(0.36989) C51B(0.36989)
 H51B(0.36989) O5A(0.64611) O6A(0.64611) N4A(0.64611) C5A(0.64611)
 H5AA(0.64611) H5AB(0.64611) H5AC(0.64611) O5B(0.35389) O6B(0.35389)
 N4B(0.35389) C5B(0.35389) H5BA(0.35389) H5BB(0.35389) H5BC(0.35389)
5.a Aromatic/amide H refined with riding coordinates:
 C11A(H11A), C21A(H21A), C41A(H41A), C51A(H51A), C11B(H11B), C21B(H21B),
 C41B(H41B), C51B(H51B)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5A(H5AA,H5AB,H5AC), C5B(H5BA,H5BB,H5BC)
;
_olex2_submission_original_sample_id cxb_CuOAcBptz_NM
_olex2_submission_special_instructions 'No special instructions were received'