Anion controlled structural and magnetic diversity in unusual mixed-bridged polynuclear Ni(II) complexes with a versatile bis(2-methoxy phenol)diamine hexadentate ligand. An experimental and theoretical magneto-structural study.
Botana, Luis; Ruiz, José; Mota, Antonio J.; Rodríguez-Diéguez, Antonio; Seco, José M; Oyarzabal, Itziar; Colacio, Enrique; Dalton transactions (Cambridge, England : 2003) 43 (2014) 13509–13524; doi:10.1039/c4dt01253d

data_7032388
_publ_section_title
;
 Anion controlled structural and magnetic diversity in unusual
 mixed-bridged polynuclear Ni(II) complexes with a versatile bis(2-methoxy
 phenol)diamine hexadentate ligand. An experimental and theoretical
 magneto-structural study.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13509
_journal_page_last               13524
_journal_paper_doi               10.1039/c4dt01253d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C44 H62 N7 Ni2 O8, C45 H64 N13 Na2 Ni2 O9'
_chemical_formula_sum            'C93 H142 N20 Na2 Ni4 O21'
_chemical_formula_weight         2157.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-06-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.256(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.938(7)
_cell_length_b                   19.592(3)
_cell_length_c                   13.763(2)
_cell_measurement_reflns_used    15380
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.34
_cell_volume                     10167(3)
_computing_cell_refinement       'Bruker smart'
_computing_data_collection       'Bruker smart'
_computing_data_reduction        'Bruker smart'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker Axs APEX automatic diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58295
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.234
_diffrn_reflns_theta_min         1.080
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4568
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         11835
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0680P)^2^+3.2740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1147
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9692
_reflns_number_total             11835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7031695
_cod_data_source_file            c4dt01253d2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               7032388
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.828
_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, All O(H) groups
2. Restrained distances
 O3A-H3AA
 0.87 with sigma of 0.01
 O1X-H1X
 0.87 with sigma of 0.01
 C16A-H3AA
 1.866552 with sigma of 0.02
 Ni1-H3AA
 2.833902 with sigma of 0.02
 C1M-H1X
 1.895444 with sigma of 0.02
 Na1-H1X
 2.962955 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(N1X) = Uiso(O1X)
4. Others
 Fixed Sof: O1X(0.5) H1X(0.5) N2X(0.5) N3X(0.5) N1X(0.5) C1M(0.5) H1MA(0.5)
 H1MB(0.5) H1MC(0.5)
 Fixed U12: N1N(0) N3N(0) N2N(0)
 Fixed U23: N1N(0) N3N(0) N2N(0)
 Fixed X: N1N(1) N3N(1) N2N(1)
 Fixed Z: N1N(0.75) N3N(0.75) N2N(0.75)
5.a Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C7B(H7BA,H7BB), C8A(H8AA,H8AB), C8B(H8BA,H8BB), C9A(H9AA,
 H9AB), C9B(H9BA,H9BB), C10A(H10C,H10D), C10B(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C5A(H5A), C5B(H5B), C12A(H12A), C12B(H12B), C14A(H14A),
 C14B(H14B)
5.c Idealised Me refined as rotating group:
 C17A(H17D,H17E,H17F), C17B(H17A,H17B,H17C), C18A(H18D,H18E,H18F), C18B(H18A,
 H18B,H18C), C21A(H21D,H21E,H21F), C21B(H21A,H21B,H21C), C31A(H31D,H31E,H31F),
 C31B(H31A,H31B,H31C), C32A(H32D,H32E,H32F), C32B(H32A,H32B,H32C), C41A(H41D,
 H41E,H41F), C41B(H41A,H41B,H41C), C1M(H1MA,H1MB,H1MC)
;
_olex2_submission_special_instructions 'No special instructions were received'