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_7032387
_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, C0.67 H3.01 O, 0.67(O), 1.33(C H4 O), N3, H2 O'
_chemical_formula_sum            'C46 H74 N10 Ni2 O12'
_chemical_formula_weight         1076.57
_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             2014-06-16
_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                 92.532(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3901(3)
_cell_length_b                   20.2174(4)
_cell_length_c                   18.9053(5)
_cell_measurement_reflns_used    1680
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.04
_cell_measurement_theta_min      2.27
_cell_volume                     5112.9(2)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'Bruker Axs APEX automatic diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0936
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30389
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.992
_diffrn_reflns_theta_min         2.015
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         11679
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0496P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7243
_reflns_number_total             11679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7031694
_cod_data_source_file            c4dt01253d2.cif
_cod_data_source_block           compound1
_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               7032387
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.806
_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, All O(H,H) groups
2. Restrained distances
 O3M-C3M
 1.4 with sigma of 0.01
 C16A-H3A
 1.870921 with sigma of 0.02
 Ni1-H3A
 2.85363 with sigma of 0.02
 C16B-H3B
 1.872654 with sigma of 0.02
 Ni2-H3B
 2.811348 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(O3W) = Uiso(C3M)
4. Others
 Fixed Sof: O2W(0.5) C3M(0.33) H3MA(0.33) H3MB(0.33) H3MC(0.33) C1M(0.67)
 H1MA(0.67) H1MB(0.67) H1MC(0.67) O3M(0.33) H3M(0.33) O3W(0.17)
5.a Riding coordinates:
 O3A(H3A), O3B(H3B), C3A(H3AA), C3B(H3BA), C5A(H5A), C5B(H5B), C12A(H12A),
 C12B(H12B), C14A(H14A), C14B(H14B), O1M(H1M), C1M(H1MA,H1MB,H1MC), O2M(H2M),
 O1W(H1WA,H1WB)
5.b Rotating group:
 C17A(H17A,H17B,H17C), C17B(H17D,H17E,H17F), C18A(H18A,H18B,H18C), C18B(H18D,
 H18E,H18F), C21A(H21A,H21B,H21C), C21B(H21D,H21E,H21F), C31A(H31A,H31B,H31C),
 C31B(H31D,H31E,H31F), C32A(H32A,H32B,H32C), C32B(H32D,H32E,H32F), C41A(H41A,
 H41B,H41C), C41B(H41D,H41E,H41F), C2M(H2MA,H2MB,H2MC)
5.c 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(H10A,H10B), C10B(H10C,H10D)
5.d Me refined with riding coordinates:
 C3M(H3MA,H3MB,H3MC)
5.e Idealised tetrahedral OH refined as rotating group:
 O3M(H3M)
;
_olex2_submission_special_instructions 'No special instructions were received'