N<sub>3</sub>-Ligated nickel(ii) diketonate complexes: synthesis, characterization and evaluation of O<sub>2</sub> reactivity.
Elsberg, Josiah G. D.; Peterson, Austin; Fuller, Amy L.; Berreau, Lisa M.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7564–7575; doi:10.1039/d0dt01338b

data_7704435
_publ_section_title
;
 N<sub>3</sub>-Ligated nickel(ii) diketonate complexes: synthesis,
 characterization and evaluation of O<sub>2</sub> reactivity.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7564
_journal_page_last               7575
_journal_paper_doi               10.1039/d0dt01338b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C42 H34 N10 Ni, 2(Cl O4), 1.5(C2 H3 N)'
_chemical_formula_sum            'C45 H38.5 Cl2 N11.5 Ni O8'
_chemical_formula_weight         997.98
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-20 deposited with the CCDC.	2020-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                87.747(3)
_cell_angle_beta                 77.340(3)
_cell_angle_gamma                77.490(3)
_cell_formula_units_Z            4
_cell_length_a                   12.2882(13)
_cell_length_b                   19.219(2)
_cell_length_c                   19.786(2)
_cell_measurement_reflns_used    9194
_cell_measurement_temperature    105
_cell_measurement_theta_max      24.988
_cell_measurement_theta_min      3.010
_cell_volume                     4450.8(8)
_computing_cell_refinement       'SAINT V8.38A (BRUKER, 2016)'
_computing_data_collection       'APEX 3 (BRUKER, 2016)'
_computing_data_reduction        'SAINT V8.38A (BRUKER, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      105.0
_diffrn_detector                 'Bruker Photon-100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            145239
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.106
_diffrn_reflns_theta_max         25.106
_diffrn_reflns_theta_min         3.011
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.5618
_exptl_absorpt_correction_T_min  0.5359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0600 before and 0.0578 after correction. The Ratio of minimum to maximum transmission is 0.9539. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       prism
_exptl_crystal_F_000             2060
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN/Et2O'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.501(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2487
_refine_ls_number_reflns         31034
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+2.5150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                27534
_reflns_number_total             31034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01338b2.cif
_cod_data_source_block           usu_lb17_sq
_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/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 7704434--7704437.cif.
;
_cod_original_cell_volume        4450.7(8)
_cod_original_formula_sum        'C45 H38.50 Cl2 N11.50 Ni O8'
_cod_database_code               7704435
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.885
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.499(8)
 0.501(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Cl2S-O7S \\sim Cl2S-O7T \\sim Cl2S-O8S \\sim Cl2S-O8T
 with sigma of 0.02
 Cl5S-O17S \\sim Cl5S-O17T \\sim Cl5S-O19S \\sim Cl5S-O19T
 with sigma of 0.02
 Cl8S-O30S \\sim Cl8S-O30T \\sim Cl8S-O31S \\sim Cl8S-O31T
 with sigma of 0.02
4. Rigid bond restraints
 C22A, C23A, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C22A \\sim C23A \\sim C24A \\sim C25A \\sim C26A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(O31S) = Uanis(O31T)
Uanis(O7T) = Uanis(O7S)
Uanis(C23A) = Uanis(C24A) = Uanis(C25A)
6. Rigid body (RIGU) restrains
 N7A, C35A, C22A, C23A, C24A, C25A, C26A, N6A, C27A, N9A, N8A, C34A, C29A,
 C42A, C37A, N10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O7T)=Sof(O8T)=1-FVAR(1)
 Sof(O7S)=Sof(O8S)=FVAR(1)
 Sof(O17T)=Sof(O19T)=1-FVAR(2)
 Sof(O17S)=Sof(O19S)=FVAR(2)
 Sof(O30T)=Sof(O31T)=1-FVAR(3)
 Sof(O30S)=Sof(O31S)=FVAR(3)
8.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A),
 C17A(H17A), C18A(H18A), C19A(H19A), C20A(H20A), C23A(H23A), C24A(H24A),
 C25A(H25A), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A), C38A(H38A),
 C39A(H39A), C40A(H40A), C41A(H41A), C2B(H2B), C3B(H3B), C4B(H4B), C9B(H9B),
 C10B(H10B), C11B(H11B), C12B(H12B), C17B(H17B), C18B(H18B), C19B(H19B),
 C20B(H20B), C23B(H23B), C24B(H24B), C25B(H25B), C30B(H30B), C31B(H31B),
 C32B(H32B), C33B(H33B), C38B(H38B), C39B(H39B), C40B(H40B), C41B(H41B),
 C2C(H2C), C3C(H3C), C4C(H4C), C9C(H9C), C10C(H10C), C11C(H11C), C12C(H12C),
 C17C(H17C), C18C(H18C), C19C(H19C), C20C(H20C), C23C(H23C), C24C(H24C),
 C25C(H25C), C30C(H30C), C31C(H31C), C32C(H32C), C33C(H33C), C38C(H38C),
 C39C(H39C), C40C(H40C), C41C(H41C), C2D(H2D), C3D(H3D), C4D(H4D), C9D(H9D),
 C10D(H10D), C11D(H11D), C12D(H12D), C17D(H17D), C18D(H18D), C19D(H19D),
 C20D(H20D), C23D(H23D), C24D(H24D), C25D(H25D), C30D(H30D), C31D(H31D),
 C32D(H32D), C33D(H33D), C38D(H38D), C39D(H39D), C40D(H40D), C41D(H41D)
8.b Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C15A(H15A,H15B,H15C), C28A(H28A,H28B,H28C), C36A(H36A,
 H36B,H36C), C7B(H7BA,H7BB,H7BC), C15B(H15D,H15E,H15F), C28B(H28D,H28E,H28F),
 C36B(H36D,H36E,H36F), C7C(H7CA,H7CB,H7CC), C15C(H15G,H15H,H15I), C28C(H28G,
 H28H,H28I), C36C(H36G,H36H,H36I), C7D(H7DA,H7DB,H7DC), C15D(H15J,H15K,H15L),
 C28D(H28J,H28K,H28L), C36D(H36J,H36K,H36L), C8S(H8SA,H8SB,H8SC), C4S(H4SA,H4SB,
 H4SC), C2S(H2SA,H2SB,H2SC), C10S(H10E,H10F,H10G), C6S(H6SA,H6SB,H6SC),
 C12S(H12E,H12F,H12G)
;
_shelx_res_checksum              12418
_shelx_fab_checksum              55216
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'