Ni(II) formate complexes with bi- and tridentate nitrogen-donor ligands: synthesis, characterization, and magnetic and thermal properties.
Rühlig, Karoline; Abylaikhan, Akerke; Aliabadi, Azar; Kataev, Vladislav; Liebing, Simon; Schwalbe, Sebastian; Trepte, Kai; Ludt, Christian; Kortus, Jens; Büchner, Bernd; Rüffer, Tobias; Lang, Heinrich; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3963–3979; doi:10.1039/c6dt04556a

data_7042343
_publ_section_title
;
 Ni(II) formate complexes with bi- and tridentate nitrogen-donor ligands:
 synthesis, characterization, and magnetic and thermal properties.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3963
_journal_page_last               3979
_journal_paper_doi               10.1039/c6dt04556a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C11 H25 N3 Ni O4, 0.5(H2 O)'
_chemical_formula_sum            'C11 H26 N3 Ni O4.5'
_chemical_formula_weight         331.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-11-25 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.006(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.8174(7)
_cell_length_b                   8.5618(4)
_cell_length_c                   13.1881(6)
_cell_measurement_reflns_used    6672
_cell_measurement_temperature    110
_cell_measurement_theta_max      28.0747
_cell_measurement_theta_min      3.0150
_cell_volume                     3043.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10743
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.023
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 2061 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.007(8)
_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     360
_refine_ls_number_reflns         4941
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    0.848
_reflns_Friedel_fraction_max     0.848
_reflns_number_gt                4739
_reflns_number_total             4941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04556a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
Adding full bibliography for 7042340--7042344.cif.

2017-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C11 H25 N3 Ni O4), H2 O'
_cod_original_formula_sum        'C22 H52 N6 Ni2 O9'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     662.11
_cod_database_code               7042343
_shelxl_version_number           2013-4
_shelx_res_checksum              5315