Syntheses, crystal structures and magnetic properties of a series of μ-phenoxo-μ1,1-carboxylato-μ1,3-carboxylato trinickel(ii) compounds.
Bhattacharya, Sagarika; Sasmal, Sujit; Carrella, Luca; Rentschler, Eva; Mohanta, Sasankasekhar; Dalton transactions (Cambridge, England : 2003) 43 (2014) 12065–12076; doi:10.1039/c4dt00862f

data_7031392
_publ_section_title
;
 Syntheses, crystal structures and magnetic properties of a series of
 \m-phenoxo-\m1,1-carboxylato-\m1,3-carboxylato trinickel(ii) compounds.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12065
_journal_page_last               12076
_journal_paper_doi               10.1039/c4dt00862f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C54 H54 N4 Ni3 O12,3(C H2 Cl2)'
_chemical_formula_sum            'C57 H60 Cl6 N4 Ni3 O12'
_chemical_formula_weight         1381.92
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-05-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.934(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9987(16)
_cell_length_b                   19.977(3)
_cell_length_c                   15.049(2)
_cell_measurement_reflns_used    5140
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.94
_cell_measurement_theta_min      2.22
_cell_volume                     3108.5(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37221
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.841
_diffrn_reflns_theta_min         1.764
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  0.8216
_exptl_absorpt_correction_T_min  0.7882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5991
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0810P)^2^+1.8460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4034
_reflns_number_total             5991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00862f2.cif
_cod_data_source_block           added_by_encifer
_cod_depositor_comments
'Adding full bibliography for 7031386--7031393.cif.'
_cod_database_code               7031392
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.775
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl5-Cl3
 1.54 with sigma of 0.02
 C9A-C8 \\sim C9B-C8
 with sigma of 0.02
 N2A-C9A \\sim N2B-C9B
 with sigma of 0.02
 N2B-C13A \\sim N2B-C10B \\sim N2A-C13B \\sim N2A-C10A
 with sigma of 0.02
 O6A-C12B \\sim O6B-C12A \\sim O6B-C11B \\sim O6A-C11A
 with sigma of 0.02
 C13B-C12B \\sim C13A-C12A \\sim C11B-C10B \\sim C11A-C10A
 with sigma of 0.02
 C30-Cl4 \\sim C30-Cl5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N2A) = Uanis(N2B)
Uanis(O6A) = Uanis(O6B)
Uanis(C10B) = Uanis(C10A)
Uanis(C13B) = Uanis(C13A)
Uanis(C12B) = Uanis(C12A)
Uanis(C11B) = Uanis(C11A)
Uiso(Cl5) = Uiso(Cl4)
4. Others
 Fixed Sof: H8AA(0.5) H8AB(0.5) H8BC(0.5) H8BD(0.5) C10B(0.5) H10A(0.5)
 H10B(0.5) C11B(0.5) H11A(0.5) H11B(0.5) C12B(0.5) H12A(0.5) H12B(0.5)
 C13B(0.5) H13A(0.5) H13B(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) C9B(0.5) H9BA(0.5)
 H9BB(0.5) N2A(0.5) O6B(0.5) Cl3(0.7) Cl5(0.15) C13A(0.5) H13C(0.5) H13D(0.5)
 C10A(0.5) H10C(0.5) H10D(0.5) C12A(0.5) H12C(0.5) H12D(0.5) C11A(0.5)
 H11C(0.5) H11D(0.5) O6A(0.5) N2B(0.5) Cl4(0.15) C29(0.35) H29A(0.35)
 H29B(0.35) C30(0.15) H30A(0.15) H30B(0.15)
5.a Riding coordinates:
 C8(H8AA,H8AB,H8BC,H8BD), C9A(H9AA,H9AB), C9B(H9BA,H9BB), C29(H29A,H29B),
 C30(H30A,H30B)
5.b Secondary CH2 refined with riding coordinates:
 C10B(H10A,H10B), C11B(H11A,H11B), C12B(H12A,H12B), C13B(H13A,H13B), C28(H28A,
 H28B), C13A(H13C,H13D), C10A(H10C,H10D), C12A(H12C,H12D), C11A(H11C,H11D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
;