The high pressure behaviour of the 3D copper carbonate framework {[Cu(CO3)2](CH6N3)2}n
Spencer, Elinor C.; Ross, Nancy L.; Angel, Ross J.; Journal of Materials Chemistry 22 (2012) 2074–; doi:10.1039/c2jm15206a

data_7207322
_publ_section_title
;
 The high pressure behaviour of the 3D copper carbonate framework
 {[Cu(CO3)2](CH6N3)2}n
;
_journal_issue                   5
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2074
_journal_paper_doi               10.1039/c2jm15206a
_journal_volume                  22
_journal_year                    2012
_chemical_formula_moiety         'C2 Cu O6, 2(C H6 N3)'
_chemical_formula_sum            'C4 H12 Cu N6 O6'
_chemical_formula_weight         303.74
_chemical_name_systematic
;
?
;
_space_group_IT_number           118
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8048(2)
_cell_length_b                   8.8048(2)
_cell_length_c                   12.0310(2)
_cell_measurement_reflns_used    3535
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.0710
_cell_measurement_theta_min      3.3795
_cell_volume                     932.70(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET)
(compiled Jan 29 2010,16:49:25)
;
_computing_data_reduction
;
Average v2.2 (Angel, 2003) www.crystal.vt.edu/crystal
Absorb Angel (2004) J. Appl. Cryst. 37:486-492
;
_computing_molecular_graphics
;
CrystalMaker V.2.0.6, CrystalMaker Software Ltd.'
;
_computing_structure_refinement
;
shelxl-97 (G.M.Sheldrick, 2008, Acta Cryst., A64,112)
WinGX (L.J Farrugia, 1999, J. Appl. Cryst., 32, 837)
;
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Oxford Diffraction, Xcalibur1 CCD'
_diffrn_measured_fraction_theta_full 0.629
_diffrn_measured_fraction_theta_max 0.629
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur1'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.948
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7095
_diffrn_reflns_reduction_process
;
Data averaged using Blessing (1987) criteria
;
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    2.379
_exptl_absorpt_correction_T_max  0.304
_exptl_absorpt_correction_T_min  0.217
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Gaussian integration over a grid
of 16 x 8 x 16 points = 2048 total grid points
Based upon method of Burnham (1966)

Data corrected for diamond-anvil cell absorption
Note that exptl_absorpt_correction_tmin and _tmax
the total correction factors applied to the intensities
The individual factors are:
range of dac transmission factors (min-max) 0.302 0.394
range of gasket transmission (min-max) 0.972 1.000
range of P media transmission (min-max) 1.000 1.000

thickness of diamond anvil 1: 1.500 mm, mu = 0.2000 mm-1
thickness of platten 1: 3.300 mm, mu = 0.0500 mm-1

thickness of diamond anvil 2: 1.500 mm, mu = 0.2000 mm-1
thickness of platten 2: 3.300 mm, mu = 0.0500 mm-1

Gasket shadowing corrections were made based upon
Gasket thickness = 145.0 microns, radius = 250.0 microns
Gasket absorption coeff = 30.00 mm-1
REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF
FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.20

Non-absorbing pressure medium
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             620
_exptl_crystal_preparation
;
Crystal mounted in a diamond-anvil cell
Crystal held under 3.95GPa of pressure
;
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.200
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.7(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         456
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0884
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1713P)^2^+1.1225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2416
_refine_ls_wR_factor_ref         0.2658
_reflns_number_gt                349
_reflns_number_total             544
_reflns_threshold_expression     'Fsqd > 2.0u(Fsqd)'
_cod_data_source_file            c2jm15206a.txt
_cod_data_source_block           Crystal_I_3.95GPa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_diffrn_radiation_probe' value 'X-ray' changed to
'x-ray' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian'
changed to 'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-4n2
_cod_database_code               7207322
_exptl_absorpt_correction_mu     2.379
_diffrn_reflns_uneti/neti        0.004