Modulation of the CO2 fixation in dinickel azacryptands.
Möller, F; Castañeda-Losada, L; Junqueira, J. R. C.; Miller, R. G.; Reback, M. L.; Mallick, B.; van Gastel, M.; Apfel, U.-P.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5680–5688; doi:10.1039/c6dt04527h

data_7041955
_publ_section_title
;
 Modulation of the CO2 fixation in dinickel azacryptands.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5680
_journal_page_last               5688
_journal_paper_doi               10.1039/c6dt04527h
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C10 H24 N6 Ni, 2(Cl O4)'
_chemical_formula_sum            'C10 H24 Cl2 N6 Ni O8'
_chemical_formula_weight         485.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-02-03 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.9793(9)
_cell_length_b                   10.8558(3)
_cell_length_c                   11.0677(4)
_cell_measurement_reflns_used    6746
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      36.5984
_cell_measurement_theta_min      2.9056
_cell_volume                     3842.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.15
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4184
_diffrn_reflns_point_group_measured_fraction_full 0.681
_diffrn_reflns_point_group_measured_fraction_max 0.648
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.189
_diffrn_reflns_theta_min         4.301
_exptl_absorpt_coefficient_mu    4.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.638
_exptl_transmission_factor_min   0.467
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2652
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+39.5549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.273
_reflns_Friedel_fraction_full    0.331
_reflns_Friedel_fraction_max     0.294
_reflns_number_gt                2581
_reflns_number_total             2652
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {b245eeae-109b-4e98-8083-0e4b39bab528}
_cod_data_source_file            c6dt04527h2.cif
_cod_data_source_block           Tren-Ni-CH3CN-2-ClO4-3_upa_fm435
_cod_depositor_comments
'Adding full bibliography for 7041952--7041960.cif.'
_cod_original_cell_volume        3842.27(19)
_cod_database_code               7041955
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.638
_shelx_estimated_absorpt_t_min   0.467
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), C1(H1A,H1B), C2(H2C,H2D), C3(H3C,H3D),
 C4(H4C,H4D), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'