Thermal and photochemical control of nitro–nitrito linkage isomerism in single-crystals of [Ni(medpt)(NO2)(η2-ONO)]
Hatcher, Lauren E.; Bigos, Edward J.; Bryant, Mathew J.; MacCready, Emily M.; Robinson, Thomas P.; Saunders, Lucy K.; Thomas, Lynne H.; Beavers, Christine M.; Teat, Simon J.; Christensen, Jeppe; Raithby, Paul R.; CrystEngComm 16 (2014) 8263–; doi:10.1039/C4CE00675E

data_7216717
_publ_section_title
;
 Thermal and photochemical control of nitro--nitrito linkage isomerism in
 single-crystals of [Ni(medpt)(NO2)(\h2-ONO)]
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              8263
_journal_paper_doi               10.1039/C4CE00675E
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98
_chemical_name_systematic
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 103.958(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            6
_cell_length_a                   7.101(5)
_cell_length_b                   23.928(5)
_cell_length_c                   10.936(5)
_cell_measurement_reflns_used    6907
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.0601
_cell_measurement_theta_min      3.0579
_cell_volume                     1803.3(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3795
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12927
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.25
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7549
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                6258
_reflns_number_total             7549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00675e2.cif
_cod_data_source_block           complex7_120K
_cod_depositor_comments
'Adding full bibliography for 7216709--7216720.cif.'
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7216717