A Simplified Extractive Metallurgy Exercise to Demonstrate Selective Extraction of Copper
Smellie, Iain A.; Abdelhamid, Yusra; Carpenter-Warren, Cameron L.; Cordes, David B.; Elliott, Clement; Lamorte, Sarah; Patterson, Iain L. J.; Sanders, William; Sandison, Iain P.; Slawin, Alexandra M. Z.; Stewart, Dominic M.; Walters, Samuel N.; Journal of Chemical Education  (2020) –; doi:10.1021/acs.jchemed.9b00996

data_1557327
_publ_section_title
;
 A Simplified Extractive Metallurgy Exercise to Demonstrate Selective
 Extraction of Copper
;
_journal_name_full               'Journal of Chemical Education'
_journal_paper_doi               10.1021/acs.jchemed.9b00996
_journal_year                    2020
_chemical_formula_moiety         'C16 H16 Cu N2 O6'
_chemical_formula_sum            'C16 H16 Cu N2 O6'
_chemical_formula_weight         395.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.790(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4484(7)
_cell_length_b                   4.8581(4)
_cell_length_c                   18.7404(15)
_cell_measurement_reflns_used    613
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      2.2
_cell_volume                     766.48(11)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material
'Olex2 (Dolomanov et al., 2009), enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 51.8800
	          2theta: -29.5400
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 51.8800
	          2theta: -29.5400
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 51.8800
	          2theta: -29.5400
;
_diffrn_measurement_device
;
SCXMini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Loop
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.060207
_diffrn_orient_matrix_UB_12      0.102374
_diffrn_orient_matrix_UB_13      0.001886
_diffrn_orient_matrix_UB_21      -0.112902
_diffrn_orient_matrix_UB_22      0.063450
_diffrn_orient_matrix_UB_23      0.159994
_diffrn_orient_matrix_UB_31      0.037752
_diffrn_orient_matrix_UB_32      -0.017634
_diffrn_orient_matrix_UB_33      0.033633
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6266
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_min         2.181
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_type              'Rigaku SCXMini'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.463
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             406
_exptl_crystal_preparation       Loop
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1400
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.6392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1119
_reflns_number_total             1400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ed9b00996_si_004.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C16 H16 Cu1 N2 O6'
_cod_database_code               1557327
_shelx_shelxl_version_number     2018/3
_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,H) groups
2. Restrained distances
 O2-H2
 0.98 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C3(H3), C4(H4)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              47383
_shelx_hkl_checksum              99903