Diazopyrazolones as weak solvent extractants for copper from ammonia leach solutions †
Emeleus, Lucy C.; Cupertino, Domenico C.; Harris, Steven G.; Owens, Susan; Parsons, Simon; Swart, Ronald M.; Tasker, Peter A.; White, David J.; Journal of the Chemical Society, Dalton Transactions  (2001) 1239–; doi:10.1039/b101780m

data_7010657
_publ_section_title
;
 Diazopyrazolones as weak solvent extractants for copper from ammonia
 leach solutions&#x200A;&#x2020;
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1239
_journal_paper_doi               10.1039/b101780m
_journal_year                    2001
_chemical_formula_moiety         '[NiL2(MeOH)2].2MeOH'
_chemical_formula_sum            'C46 H60 N6 Ni O6'
_chemical_formula_weight         851.71
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                76.735(6)
_cell_angle_beta                 79.025(6)
_cell_angle_gamma                77.539(7)
_cell_formula_units_Z            2
_cell_length_a                   10.5849(12)
_cell_length_b                   14.896(2)
_cell_length_c                   15.153(2)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     2245.6(5)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      220(2)
_diffrn_measurement_device
; 
? 
;
_diffrn_measurement_method       Omega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            8035
_diffrn_reflns_theta_max         70.09
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        -2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.065
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         7967
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_obs          0.0469
_refine_ls_shift/esd_max         -0.034
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+1.5324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1335
_refine_ls_wR_factor_obs         0.1252
_reflns_number_observed          6602
_reflns_number_total             7972
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b101780m.txt
_cod_data_source_block           le214d
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+1.5324P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+1.5324P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2245.6(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010657