Preorganized tridentate analogues of mixed hydroxyoxime/carboxylate nickel extractants.
Roebuck, James W.; Turkington, Jennifer R.; Rogers, David M.; Bailey, Philip J.; Griffin, Violina; Fischmann, Adam J.; Nichol, Gary S.; Pelser, Max; Parsons, Simon; Tasker, Peter A.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 3734–3742; doi:10.1039/c5dt04288g

data_7038015
_publ_section_title
;
 Preorganized tridentate analogues of mixed hydroxyoxime/carboxylate
 nickel extractants.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3734
_journal_page_last               3742
_journal_paper_doi               10.1039/c5dt04288g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C35.90 N4 Ni1 O6 S2'
_chemical_formula_sum            'C35.9 N4 Ni O6 S2'
_chemical_formula_weight         706.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2015-10-27 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 130.464(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5566(9)
_cell_length_b                   15.2328(2)
_cell_length_c                   13.6475(5)
_cell_measurement_reflns_used    13572
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     3567.7(4)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33034
_diffrn_reflns_theta_full        25.139
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         2.926
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1405.600
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.153
_refine_diff_density_max         1.17
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.3724
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         8860
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.0004533
_refine_ls_shift/su_mean         0.0000210
_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: 
 459. 668. 332. 82.9 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1284
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1284
_reflns_limit_h_max              23
_reflns_limit_h_min              -30
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7407
_reflns_number_total             8881
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.73
_oxford_diffrn_Wilson_scale      0.24
_oxford_refine_ls_r_factor_ref   0.0757
_oxford_refine_ls_scale          2.024(9)
_oxford_reflns_number_all        8860
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            c5dt04288g2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7038007--7038015.cif.
;
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C35.90 N4 Ni1 O6 S2'
_cod_database_code               7038015
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONT NI(1, U'S) UNTIL C(441) 
CONT C(4420, U[ISO]) UNTIL C(4431) 
CONT C(421, U'S) 
CONT C(520, U[ISO]) UNTIL C(221) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST 1.54, 0.005 = C(4420) TO C(4430) 
DIST 1.54, 0.005 = C(4420) TO C(4440) 
DIST 1.54, 0.005 = C(4420) TO C(4450) 
ANGLE 109, 1 = C(42) TO C(4420) TO C(4430) 
ANGLE 109, 1 = C(42) TO C(4420) TO C(4440) 
ANGLE 109, 1 = C(42) TO C(4420) TO C(4450) 
ANGLE 109, 1 = C(4430) TO C(4420) TO C(4440) 
ANGLE 109, 1 = C(4440) TO C(4420) TO C(4450) 
ANGLE 109, 1 = C(4450) TO C(4420) TO C(4430) 
DIST 1.54, 0.005 = C(4421) TO C(4431) 
DIST 1.54, 0.005 = C(4421) TO C(4441) 
DIST 1.54, 0.005 = C(4421) TO C(4451) 
ANGLE 109, 1 = C(42) TO C(4421) TO C(4431) 
ANGLE 109, 1 = C(42) TO C(4421) TO C(4441) 
ANGLE 109, 1 = C(42) TO C(4421) TO C(4451) 
ANGLE 109, 1 = C(4431) TO C(4421) TO C(4441) 
ANGLE 109, 1 = C(4441) TO C(4421) TO C(4451) 
ANGLE 109, 1 = C(4451) TO C(4421) TO C(4431) 
DISTANCE 1.230000 , 0.050000 = N(221) TO O(231) 
DISTANCE 1.230000 , 0.050000 = N(220) TO O(230) 
DISTANCE 1.230000 , 0.050000 = N(221) TO O(241) 
DISTANCE 1.230000 , 0.050000 = N(220) TO O(240) 
ANGLE 123, 1 = O(231) TO N(221) TO O(241) 
ANGLE 123, 1 = O(230) TO N(220) TO O(240) 
ANGLE 118.5, 1 = C(22) TO N(221) TO O(231) 
ANGLE 118.5, 1 = C(22) TO N(221) TO O(241) 
ANGLE 118.5, 1 = C(22) TO N(220) TO O(230) 
ANGLE 118.5, 1 = C(22) TO N(220) TO O(240) 
DISTANCE 1.450000 , 0.050000 = N(221) TO C(22) 
DISTANCE 1.450000 , 0.050000 = N(220) TO C(22) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.530000 , 0.050000 = C(42) TO C(4421) 
DISTANCE 1.530000 , 0.050000 = C(42) TO C(4420) 
END                                                                             
;