Tuning the coordination chemistry of a Cu(ii) complex at high-pressure.
Gould, Jamie A.; Rosseinsky, Matthew J.; Moggach, Stephen A.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 5464–5467; doi:10.1039/c2dt12302a

data_7018877
_publ_section_title
;
 Tuning the coordination chemistry of a Cu(ii) complex at high-pressure.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5464
_journal_page_last               5467
_journal_paper_doi               10.1039/c2dt12302a
_journal_volume                  41
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C4 H9 Cu1 N1 O6'
_chemical_formula_sum            'C4 H9 Cu N O6'
_chemical_formula_weight         230.66
_chemical_name_common            CuAsp
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             11-07-11
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 91.332(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9747(5)
_cell_length_b                   9.5739(6)
_cell_length_c                   7.2465(11)
_cell_measurement_reflns_used    1340
_cell_measurement_temperature    293
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     622.47(11)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_pressure         5900000
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.420
_diffrn_measured_fraction_theta_max 0.396
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ' synchrotron'
_diffrn_radiation_wavelength     0.47620
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            2505
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         30.515
_diffrn_reflns_theta_min         3.112
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.500
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.50
_refine_ls_abs_structure_details 'Flack (1983), 322 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.26(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9640
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         714
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.0002175
_refine_ls_shift/su_mean         0.0000328
_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:
3.98 4.18 0.887
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0642
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0642
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              4
_reflns_limit_l_min              0
_reflns_number_gt                582
_reflns_number_total             723
_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   0.0371
_oxford_refine_ls_scale          0.2324(2)
_oxford_reflns_number_all        714
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'ceth06 in C2'
_cod_data_source_file            c2dt12302a.txt
_cod_data_source_block           ceth06
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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      'C 2'
_cod_original_formula_sum        'C4 H9 Cu1 N1 O6'
_cod_database_code               7018877
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S
CONT CU(1, U'S)
CONT C(1, U[ISO]) UNTIL N(1)
CONT ENANTIO
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S)
RIDE O ( 5,X'S) H ( 51,X'S) H ( 52,X'S)
RIDE O ( 6,X'S) H ( 61,X'S) H ( 62,X'S)
RIDE N ( 1,X'S) H ( 11,X'S) H ( 12,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
DIST 1.292, 0.01 = C(1) TO O(1)
DIST 1.232, 0.01 = C(1) TO O(2)
DIST 1.525, 0.01 = C(1) TO C(2)
DIST 1.489, 0.01 = C(2) TO N(1)
DIST 1.514, 0.01 = C(2) TO C(3)
DIST 1.528, 0.01 = C(3) TO C(4)
DIST 1.280, 0.01 = C(4) TO O(3)
DIST 1.239, 0.01 = C(4) TO O(4)
ANGL 123,1= O(2) TO C(1) TO O(1)
ANGL 118,1= C(2) TO C(1) TO O(1)
ANGL 120,1= C(2) TO C(1) TO O(2)
ANGL 109,1= C(1) TO C(2) TO N(1)
ANGL 110,1= C(3) TO C(2) TO N(1)
ANGL 110,1= C(3) TO C(2) TO C(1)
ANGL 115,1= C(4) TO C(3) TO C(2)
ANGL 124,1= O(4) TO C(4) TO O(3)
ANGL 114,1= C(3) TO C(4) TO O(3)
ANGL 122,1= C(3) TO C(4) TO O(4)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM DELU START (DO NOT REMOVE THIS LINE)
VIBR .0, 0.00200 = O(1) TO C(1)
VIBR .0, 0.00200 = O(2) TO C(1)
VIBR .0, 0.00200 = O(3) TO C(4)
VIBR .0, 0.00200 = O(4) TO C(4)
VIBR .0, 0.00200 = N(1) TO C(2)
VIBR .0, 0.00200 = C(1) TO C(2)
VIBR .0, 0.00500 = O(2) TO O(1)
VIBR .0, 0.00500 = C(2) TO O(1)
VIBR .0, 0.00500 = C(2) TO O(2)
VIBR .0, 0.00200 = C(2) TO C(3)
VIBR .0, 0.00500 = N(1) TO C(1)
VIBR .0, 0.00500 = C(3) TO C(1)
VIBR .0, 0.00500 = C(3) TO N(1)
VIBR .0, 0.00200 = C(3) TO C(4)
VIBR .0, 0.00500 = C(4) TO C(2)
VIBR .0, 0.00500 = O(3) TO C(3)
VIBR .0, 0.00500 = O(4) TO C(3)
VIBR .0, 0.00500 = O(4) TO O(3)
REM DELU END (DO NOT REMOVE THIS LINE)
REM THERMSIM START (DO NOT REMOVE THIS LINE)
U(IJ) .0, 0.08000 = O(1) TO C(1)
U(IJ) .0, 0.08000 = O(2) TO C(1)
U(IJ) .0, 0.08000 = O(3) TO C(4)
U(IJ) .0, 0.08000 = O(4) TO C(4)
U(IJ) .0, 0.08000 = N(1) TO C(2)
U(IJ) .0, 0.04000 = C(1) TO C(2)
U(IJ) .0, 0.04000 = C(2) TO C(3)
U(IJ) .0, 0.04000 = C(3) TO C(4)
REM THERMSIM END (DO NOT REMOVE THIS LINE)
END
;