Supercolossal Uniaxial Negative Thermal Expansion in Chloranilic Acid Pyrazine, CA-Pyz
Liu, Huiyu; Gutmann, Matthias J.; Stokes, Harold T.; Campbell, Branton J.; Evans, Ivana Radosavljevic; Evans, John S. O.; Chemistry of Materials 31 (2019) 4514–; doi:10.1021/acs.chemmater.9b01135

data_4003064
_publ_section_title
;
 Supercolossal Uniaxial Negative Thermal Expansion in Chloranilic Acid
 Pyrazine, CA-Pyz
;
_journal_issue                   12
_journal_name_full               'Chemistry of Materials'
_journal_page_first              4514
_journal_paper_doi               10.1021/acs.chemmater.9b01135
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         'C10 H6 Cl2 N2 O4'
_chemical_formula_sum            'C10 H6 Cl2 N2 O4'
_chemical_formula_weight         289.07
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                81.926(8)
_cell_angle_beta                 81.568(8)
_cell_angle_gamma                76.993(8)
_cell_formula_units_Z            1
_cell_length_a                   4.7821(5)
_cell_length_b                   5.8258(6)
_cell_length_c                   10.7018(10)
_cell_measurement_reflns_used    914
_cell_measurement_temperature    150
_cell_measurement_theta_max      33.5975
_cell_measurement_theta_min      2.1104
_cell_volume                     285.57(5)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3060
_diffrn_reflns_theta_full        25.371
_diffrn_reflns_theta_max         33.382
_diffrn_reflns_theta_min         3.612
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             146
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.80
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1949
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.0001602
_refine_ls_shift/su_mean         0.0000156
_refine_ls_structure_factor_coef Fsqd
_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: 
 0.163E+05 -0.119E+05 0.134E+05 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1978
_refine_ls_wR_factor_gt          0.1836
_refine_ls_wR_factor_ref         0.1836
_reflns_limit_h_max              7
_reflns_limit_h_min              -6
_reflns_limit_k_max              7
_reflns_limit_k_min              -8
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_gt                1949
_reflns_number_total             1460
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0760
_oxford_refine_ls_scale          18(2)
_oxford_reflns_number_all        3054
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            cm9b01135_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        285.57(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4003064