Pushing the limits of magnetic anisotropy in trigonal bipyramidal Ni(ii)
Marriott, Katie E. R.; Bhaskaran, Lakshmi; Wilson, Claire; Medarde, Marisa; Ochsenbein, Stefan T.; Hill, Stephen; Murrie, Mark; Chem. Sci. 6 (2015) 6823–; doi:10.1039/C5SC02854J

data_1530396
_publ_section_title
;
 Pushing the limits of magnetic anisotropy in trigonal bipyramidal Ni(ii)
;
_journal_issue                   12
_journal_name_full               'Chem. Sci.'
_journal_page_first              6823
_journal_paper_doi               10.1039/C5SC02854J
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C14 H30 Cl3 N4 Ni, Cl O4'
_chemical_formula_sum            'C14 H30 Cl4 N4 Ni O4'
_chemical_formula_weight         518.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-15 deposited with the CCDC.
2015-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3629(16)
_cell_length_b                   12.8888(19)
_cell_length_c                   13.1011(18)
_cell_measurement_reflns_used    4673
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.28
_cell_volume                     2087.6(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12167
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.580
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1293 before and 0.1087 after correction.
The Ratio of minimum to maximum transmission is 0.7465.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.16(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3646
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0364P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.913
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.940
_reflns_number_gt                3254
_reflns_number_total             3646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02854j2.cif
_cod_data_source_block           km684rc_0m
_cod_depositor_comments          'Adding full bibliography for 1530396.cif.'
_cod_database_code               1530396
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.84(3) 0.16(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b),
 C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b), C12(H12a,H12b),
 C13(H13a,H13b)
3.b Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C14(H14a,H14b,H14c)
;
_shelx_res_checksum              40911
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'