Anion-mediated bio-relevant catalytic activity of dinuclear nickel(ii) complexes derived from an end-off compartmental ligand.
Chakraborty, Tonmoy; Mukherjee, Somali; Dasgupta, Sanchari; Biswas, Biplab; Das, Debasis; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2772–2784; doi:10.1039/c8dt04631j

data_7048710
_publ_section_title
;
 Anion-mediated bio-relevant catalytic activity of dinuclear nickel(ii)
 complexes derived from an end-off compartmental ligand.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2772
_journal_page_last               2784
_journal_paper_doi               10.1039/c8dt04631j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C25 H37 N4 Ni2 O6 3+, 3(N O3 1-), 3.5(H2 O)'
_chemical_formula_sum            'C25 H44 N7 Ni2 O18.5'
_chemical_formula_weight         863.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-21 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.538(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.755(3)
_cell_length_b                   11.780(2)
_cell_length_c                   20.929(4)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.529
_cell_measurement_theta_min      1.032
_cell_volume                     3660.6(12)
_computing_cell_refinement       'BRUKER APEX II'
_computing_data_collection       'BRUKER APEX II'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2016/1 (Sheldrick, 2016)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22849
_diffrn_reflns_point_group_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        23.529
_diffrn_reflns_theta_max         23.529
_diffrn_reflns_theta_min         1.032
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0845 before and 0.0534 after correction.
The Ratio of minimum to maximum transmission is 0.7377.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   0.827
_exptl_transmission_factor_min   0.715
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.56(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         9758
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+0.2326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.704
_reflns_Friedel_fraction_full    0.787
_reflns_Friedel_fraction_max     0.787
_reflns_number_gt                7467
_reflns_number_total             9758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04631j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7048710--7048712.cif.'
_cod_original_formula_sum        'C25 H44 N7 Ni2 O18.50'
_cod_database_code               7048710
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.44(2)
 0.56(2)
2. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 O6W-H6WA = O6W-H6WB
 0.85 with sigma of 0.02
 H6WA-H6WB
 1.36 with sigma of 0.02
 C5-C24 = C5-C24A = C5-C25 = C5-C25A
 1.5 with sigma of 0.02
 C9-N1 \\sim N1-C9B
 with sigma of 0.02
 C10B-C11 \\sim C11-C10
 with sigma of 0.02
 C10-C11 \\sim C11-C10B
 with sigma of 0.02
 C10B-C9B \\sim C10-C9
 with sigma of 0.02
 C9-C10 \\sim C9B-C10B
 with sigma of 0.02
 C55A-C35 \\sim C35-C54A
 with sigma of 0.02
 O18-N13 \\sim O19-N13 \\sim O17-N13
 with sigma of 0.02
 C47-C48 \\sim C47B-C48B
 with sigma of 0.02
 C48-C47 \\sim C47B-C48B
 with sigma of 0.02
 N5-C47 \\sim N5-C47B
 with sigma of 0.02
 C48B-C47B \\sim C48-C47
 with sigma of 0.02
 C49-C48B \\sim C49-C48
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C9B)
Uanis(C10B) = Uanis(C10)
Uanis(C24A) = Uanis(C24)
Uiso(O17A) = Uiso(O17W)
Uanis(O1AA) = Uanis(O21)
Uanis(O2) = Uanis(O20)
Uanis(O22) = Uanis(O0AA)
5. Others
 Sof(O0AA)=Sof(O2)=Sof(O1AA)=1-FVAR(1)
 Sof(O20)=Sof(O21)=Sof(O22)=FVAR(1)
 Fixed Sof: C9(0.67) H9A(0.67) H9B(0.67) H35A(0.4) H35(0.6) O13W(0.5)
 H13A(0.5) H13B(0.5) H5A(0.5) H5B(0.5) O17W(0.5) H17C(0.5) H17D(0.5) O13A(0.5)
 H13C(0.5) H13D(0.5) O17A(0.5) H17E(0.5) H17F(0.5) C47(0.75) H47A(0.75)
 H47B(0.75) C48(0.75) H48A(0.75) H48B(0.75) C48B(0.25) H48C(0.25) H48D(0.25)
 C47B(0.25) H47C(0.25) H47D(0.25) C54A(0.4) H54A(0.4) H54B(0.4) H54C(0.4)
 C55(0.6) H55A(0.6) H55B(0.6) H55C(0.6) C54(0.6) H54D(0.6) H54E(0.6) H54F(0.6)
 C55A(0.4) H55D(0.4) H55E(0.4) H55F(0.4) C10(0.67) H10A(0.67) H10B(0.67)
 C9B(0.33) H9BA(0.33) H9BB(0.33) C10B(0.33) H10C(0.33) H10D(0.33) C24(0.5)
 H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C24A(0.5)
 H24D(0.5) H24E(0.5) H24F(0.5) C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5)
6.a Everything fixed:
 H2WA, H2WB, H3WA, H3WB, H4WA, H4WB, H5WB, H9WA, H9WB, H12A, H12B
6.b Riding coordinates:
 O1W(H1WA,H1WB), O5W(H5WA), O11W(H11A,H11B), O13W(H13A,H13B), O14W(H14A,H14B),
 O17W(H17C,H17D), O13A(H13C,H13D), O15W(H15A,H15B), O16W(H16A,H16B), O17A(H17E,
 H17F), C55A(H55D,H55E,H55F), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F)
6.c Rotating group:
 O7W(H7WA,H7WB), O8W(H8WA,H8WB), O10W(H10E,H10F)
6.d Ternary CH refined with riding coordinates:
 C35(H35A), C35(H35), C5(H5A), C5(H5B)
6.e Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B), C39(H39A,H39B), C40(H40A,H40B),
 C47(H47A,H47B), C48(H48A,H48B), C48B(H48C,H48D), C47B(H47C,H47D), C10(H10A,
 H10B), C9B(H9BA,H9BB), C10B(H10C,H10D)
6.f Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C20(H20), C21(H21), C22(H22), C23(H23), C33(H33), C36(H36), C38(H38), C42(H42),
  C43(H43), C44(H44), C45(H45), C46(H46), C50(H50), C51(H51), C52(H52), C53(H53)
6.g Idealised Me refined as rotating group:
 C54A(H54A,H54B,H54C), C55(H55A,H55B,H55C), C54(H54D,H54E,H54F)
;
_shelx_res_checksum              94191
_olex2_submission_special_instructions 'No special instructions were received'