Both end-on and end-to-end azide bridged tetranuclear ferromagnetic nickel(II) Schiff base complex
Chattopadhyay, Shouvik; Bhattacharyya, Anik; Das, Mithun; Bauza, Antonio; Herrero, Santiago; González-Prieto, Rodrigo; Frontera, Antonio; New J. Chem. 41 (2017) 13585–13592; doi:10.1039/C7NJ00852J

data_7056587
_publ_section_title
;
 Both end-on and end-to-end azide bridged tetranuclear ferromagnetic
 nickel(II) Schiff base complex
;
_journal_issue                   22
_journal_name_full               'New J. Chem.'
_journal_page_first              13585
_journal_page_last               13592
_journal_paper_doi               10.1039/C7NJ00852J
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C52 H80 Cl N17 Ni4 O14, C H3 O H'
_chemical_formula_sum            'C53 H84 Cl N17 Ni4 O15'
_chemical_formula_weight         1469.59
_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_method           SHELXL-2014/7
_audit_update_record
;
2017-05-21 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.24(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.494(7)
_cell_length_b                   21.318(3)
_cell_length_c                   14.593(5)
_cell_measurement_reflns_used    3530
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.8770
_cell_measurement_theta_min      2.9390
_cell_volume                     3333(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37853
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.867
_diffrn_reflns_theta_min         2.972
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       Block
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
SQUEEZE was used to remove the contributions of one solvent methanol molecule.
;
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 5319 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         15355
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.7916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.835
_reflns_number_gt                13149
_reflns_number_total             15355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00852j2.cif
_cod_data_source_block           Complex
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Analytical' changed to
'analytical' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7056587
_alert_response
;
Alert c CHEMW03, PLAT094, Alert G FORMU01, CELLZ01, PLAT041, PLAT042, PLATO68, for difference in calculated and reported Values for formula, molecular mass, absorption coefficient and F000.
Response
One methanol molecule was present as the solvent molecule which was 
removed using SQUEEZE. Thus four hydrogen atoms, one carbon atom and one oxygen atom of methanol molecule were added to the chemical formula to adjust 
the density, molecular mass and F000 value. 
Results in the chemical_formula_moiety 
C52 H80 Cl N17 Ni4 O14, C H3 O H.
;
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.710
_shelx_estimated_absorpt_t_max   0.792
_shelx_res_checksum              41920