Pressure-and Temperature Induced Phase Transitions, Piezochromism, NLC Behaviour and Pressure Controlled Jahn-Teller Switching in a Cu-based Framework
McMonagle, Charlie; Comar, Priyanka; Nichol, Gary Stephen; Allan, David Robert; Barreda-Argūeso, José A; Gonzalez, Jesus Antonio; Rodriguez, Fernando; Valiente, Rafael; Turner, Gemma; Brechin, Euan K.; Moggach, Stephen A.; Chemical Science  (2020) –; doi:10.1039/D0SC03229H

data_1558705
_publ_section_title
;
 Pressure-and Temperature Induced Phase Transitions, Piezochromism, NLC
 Behaviour and Pressure Controlled Jahn-Teller Switching in a Cu-based
 Framework
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03229H
_journal_year                    2020
_chemical_formula_moiety         'C36 H32 Cu2 N4 O8'
_chemical_formula_sum            'C36 H32 Cu2 N4 O8'
_chemical_formula_weight         1551.53
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-10
_audit_creation_method           CRYSTALS_ver_14.61_build_5965
_audit_update_record
;
2020-06-09 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   49.169(3)
_cell_length_b                   49.169(3)
_cell_length_c                   7.7897(5)
_cell_measurement_reflns_used    5751
_cell_measurement_temperature    293
_cell_measurement_theta_max      14
_cell_measurement_theta_min      2
_cell_volume                     16309.3(18)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.709
_diffrn_measured_fraction_theta_max 0.705
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.111
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            10639
_diffrn_reflns_theta_full        20.109
_diffrn_reflns_theta_max         20.731
_diffrn_reflns_theta_min         1.435
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7164
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.96
_refine_diff_density_min         -3.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         1366
_refine_ls_number_restraints     236
_refine_ls_R_factor_all          0.2815
_refine_ls_R_factor_gt           0.1966
_refine_ls_shift/su_max          0.0035154
_refine_ls_shift/su_mean         0.0001623
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.87 1.41 0.956 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4126
_refine_ls_wR_factor_gt          0.2282
_refine_ls_wR_factor_ref         0.2282
_reflns_limit_h_max              20
_reflns_limit_h_min              -47
_reflns_limit_k_max              48
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                1366
_reflns_number_total             2642
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.47
_oxford_diffrn_Wilson_scale      1363.18
_oxford_refine_ls_r_factor_ref   0.1966
_oxford_refine_ls_scale          0.0252(4)
_oxford_reflns_number_all        2575
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'LATE06_0m in R-3'
_cod_data_source_file            d0sc03229h2.cif
_cod_data_source_block           MeOH_334_Syn
_cod_original_cell_volume        16310(2)
_cod_original_sg_symbol_Hall     '-R 3 '
_cod_original_sg_symbol_H-M      'R -3 '
_cod_database_code               1558705