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_1550193
_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         'C37 H32 N6 Ni, 2(C4 H8 O)'
_chemical_formula_sum            'C45 H48 N6 Ni O2'
_chemical_formula_weight         763.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                71.802(3)
_cell_angle_beta                 84.699(4)
_cell_angle_gamma                79.232(4)
_cell_formula_units_Z            2
_cell_length_a                   11.8068(14)
_cell_length_b                   13.0124(15)
_cell_length_c                   13.3226(15)
_cell_measurement_reflns_used    4589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.99
_cell_measurement_theta_min      2.21
_cell_volume                     1908.9(4)
_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    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1151
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28953
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.802
_diffrn_reflns_theta_max         24.802
_diffrn_reflns_theta_min         2.380
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1353 before and 0.0621 after correction. The Ratio of minimum to maximum transmission is 0.8581. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orange
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       needle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0360P)^2^+1.1887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4446
_reflns_number_total             6541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03719a2.cif
_cod_data_source_block           mo_0479_anderson_mu_0m
_cod_database_code               1550193
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C52(H52A,
 H52B), C54(H54A,H54B), C53(H53A,H53B), C51(H51A,H51B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C26(H26), C25(H25), C14(H14), C40(H40), C39(H39), C16(H16),
 C31(H31), C23(H23), C37(H37), C17(H17), C35(H35), C41(H41), C44(H44), C20(H20),
  C15(H15), C28(H28), C32(H32), C36(H36), C38(H38), C22(H22), C19(H19),
 C29(H29), C42(H42), C43(H43)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              1093
_olex2_submission_special_instructions 'No special instructions were received'