Reversible Homolytic Activation of Water via Metal-Ligand Cooperativity in a T-Shaped Ni(II) Complex
Chang, Mu-Chieh; Jesse, Kate A.; Filatov, Alexander S.; Anderson, John S.; Chemical Science  (2019) –; doi:10.1039/C8SC03719A

data_1550192
_publ_section_title
;
 Reversible Homolytic Activation of Water via Metal-Ligand Cooperativity
 in a T-Shaped Ni(II) Complex
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC03719A
_journal_year                    2019
_chemical_formula_moiety         '4(C32 H26 N5 Ni), C7 H7'
_chemical_formula_sum            'C135 H111 N20 Ni4'
_chemical_formula_weight         2248.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-07 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.099(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.6944(17)
_cell_length_b                   7.3064(5)
_cell_length_c                   28.2539(17)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.35
_cell_volume                     5448.6(6)
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            43574
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.156
_diffrn_reflns_theta_min         2.250
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1329 before and 0.0612 after correction.
The Ratio of minimum to maximum transmission is 0.8916.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       plate
_exptl_crystal_F_000             2346
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 3838 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         11737
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0298P)^2^+3.2367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.958
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                10141
_reflns_number_total             11737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03719a2.cif
_cod_data_source_block           mo_0587_mu415_0m
_cod_database_code               1550192
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.755
_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) groups
2. Others
 Fixed Sof: C431(0.5) H43A(0.5) H43B(0.5) H43C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C201(H201), C191(H191), C231(H231), C221(H221), C252(H252), C192(H192),
 C261(H261), C251(H251), C232(H232), C222(H222), C202(H202), C312(H312),
 C132(H132), C372(H372), C262(H262), C362(H362), C352(H352), C171(H171),
 C382(H382), C172(H172), C162(H162), C152(H152), C321(H321), C142(H142),
 C161(H161), C141(H141), C392(H392), C391(H391), C131(H131), C281(H281),
 C351(H351), C282(H282), C322(H322), C151(H151), C381(H381), C311(H311),
 C361(H361), C292(H292), C291(H291), C371(H371), C411(H411), C401(H401)
3.b Idealised Me refined as rotating group:
 C241(H24A,H24B,H24C), C242(H24D,H24E,H24F), C331(H33A,H33B,H33C), C332(H33D,
 H33E,H33F), C431(H43A,H43B,H43C)
;
_shelx_res_checksum              77899
_olex2_submission_special_instructions 'No special instructions were received'