Efficient alkane hydroxylation catalysis of nickel(ii) complexes with oxazoline donor containing tripodal tetradentate ligands.
Terao, Ikumi; Horii, Sena; Nakazawa, Jun; Okamura, Masaya; Hikichi, Shiro; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6108–6118; doi:10.1039/d0dt00733a

data_7704094
_publ_section_title
;
 Efficient alkane hydroxylation catalysis of nickel(ii) complexes with
 oxazoline donor containing tripodal tetradentate ligands.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6108
_journal_page_last               6118
_journal_paper_doi               10.1039/d0dt00733a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         ' C25 H36 Cl N4 Ni O6, C24 H20 B '
_chemical_formula_sum            'C49 H56 B Cl N4 Ni O6'
_chemical_formula_weight         901.93
_chemical_name_common
'[(3-chlorobenzoato)aquatris{(4,4-dimethyloxazolin-2-yl)methyl}aminenickel(II)]tetraphenylborate'
_chemical_name_systematic        '[Ni(mCBA)(TOAMe2)(OH2)](BPh4)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-02-13 deposited with the CCDC.	2020-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   63.3792(17)
_cell_length_b                   58.8576(15)
_cell_length_c                   9.7929(2)
_cell_measurement_reflns_used    21176
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4815
_cell_measurement_theta_min      1.5258
_cell_volume                     36530.9(15)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction
'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2002)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 54.8475
	          2theta: -25.1967
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 54.8475
	          2theta: -25.1967
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 54.8475
	          2theta: -25.1967

;
_diffrn_measurement_device
;
Saturn70 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0962
_diffrn_orient_matrix_UB_12      -0.0338
_diffrn_orient_matrix_UB_13      -0.0062
_diffrn_orient_matrix_UB_21      0.0057
_diffrn_orient_matrix_UB_22      -0.0159
_diffrn_orient_matrix_UB_23      -0.0014
_diffrn_orient_matrix_UB_31      -0.0005
_diffrn_orient_matrix_UB_32      -0.0016
_diffrn_orient_matrix_UB_33      0.0157
_diffrn_radiation_detector       CCD
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       82
_diffrn_reflns_limit_h_min       -80
_diffrn_reflns_limit_k_max       76
_diffrn_reflns_limit_k_min       -76
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            83891
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.4815
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         1.526
_diffrn_source_current           60.0000
_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.9524
_exptl_absorpt_correction_T_min  0.8348
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;Numerical (Based on real shape of the crystal) absorption
correction was parformed on CrystalClear (Rigaku Inc., 2007)
with FS_ABSCOR method.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       needle
_exptl_crystal_F_000             15232
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 8191 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         20846
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.0454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                19997
_reflns_number_total             20846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00733a2.cif
_cod_data_source_block           shelx_CCDC4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Numerical' was
changed to 'numerical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 

 Adding full bibliography for 7704090--7704094.cif.
;
_cod_original_formula_sum        'C49 H56 B Cl N4 Ni O6  '
_cod_database_code               7704094
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              76430