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_1550191
_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         'C32 H26 N5 Ni, C20 H30 Co'
_chemical_formula_sum            'C52 H56 Co N5 Ni'
_chemical_formula_weight         868.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2018-08-07 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.630(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6597(7)
_cell_length_b                   16.9613(11)
_cell_length_c                   12.2584(8)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.21
_cell_volume                     2167.1(2)
_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: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1890
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53581
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.370
_diffrn_reflns_theta_min         2.213
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0957 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.9198.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 4811 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         10753
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+1.2664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                10284
_reflns_number_total             10753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03719a2.cif
_cod_data_source_block           mo_0430_anderson_mu_0m
_cod_database_code               1550191
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.463(17)
 0.537(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C39(H39), C23(H23), C28(H28), C37(H37), C26(H26), C25(H25),
 C32(H32), C19(H19), C22(H22), C35(H35), C29(H29), C36(H36), C15(H15), C14(H14),
  C16(H16), C13(H13), C20(H20), C31(H31), C38(H38)
3.b Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C24(H24A,H24B,
 H24C), C50(H50A,H50B,H50C), C60(H60A,H60B,H60C), C56(H56A,H56B,H56C), C58(H58A,
 H58B,H58C), C47(H47A,H47B,H47C), C57(H57A,H57B,H57C), C49(H49A,H49B,H49C),
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              11508
_olex2_submission_special_instructions 'No special instructions were received'