A family of [Ni8] cages templated by μ6-peroxide from dioxygen activation
Perivolaris, Alexandros; Stoumpos, Constantinos C.; Karpinska, Jolanta; Ryder, Alan G.; Frost, Jamie M.; Mason, Kevin; Prescimone, Alessandro; Slawin, Alexandra M. Z.; Kessler, Vadim G.; Mathieson, Jennifer S.; Cronin, Leroy; Brechin, Euan K.; Papaefstathiou, Giannis S.; Inorg. Chem. Front. 1 (2014) 487–; doi:10.1039/C4QI00048J

data_4348218
_publ_section_title
;
 A family of [Ni8] cages templated by \m6-peroxide from dioxygen
 activation
;
_journal_issue                   6
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              487
_journal_paper_doi               10.1039/C4QI00048J
_journal_volume                  1
_journal_year                    2014
_chemical_compound_source        G.Papaefstathiou
_chemical_formula_moiety         '[Ni5(aboH)6(abo)2].4MeOH.1CH2Cl2'
_chemical_formula_sum            'C117 H112 Cl2 N8 Ni5 O20'
_chemical_formula_weight         2314.67
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             12-07-19
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                98.686(3)
_cell_angle_beta                 99.661(3)
_cell_angle_gamma                90.904(3)
_cell_formula_units_Z            1
_cell_length_a                   12.8976(6)
_cell_length_b                   13.0924(6)
_cell_length_c                   16.4651(6)
_cell_measurement_reflns_used    23087
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      73.8570
_cell_measurement_theta_min      2.7544
_cell_volume                     2707.0(2)
_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    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.1107
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            54794
_diffrn_reflns_theta_full        73.953
_diffrn_reflns_theta_max         73.953
_diffrn_reflns_theta_min         2.756
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.007
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63551
_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            Orange
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1204
_exptl_crystal_recrystallization_method
;
Et2O diffusion of a MeOH/DCM solution.
;
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.71
_refine_diff_density_min         -0.74
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9640
_refine_ls_hydrogen_treatment    'see above notes'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         9648
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.0053546
_refine_ls_shift/su_mean         0.0000614
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.390E+04 0.651E+04 0.406E+04 0.173E+04 383.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2087
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.2087
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7753
_reflns_number_total             9656
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.87
_oxford_diffrn_Wilson_scale      0.09
_oxford_refine_ls_r_factor_ref   0.0829
_oxford_refine_ls_scale          3.92(6)
_oxford_reflns_number_all        9648
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'eb1089 in P-1'
_cod_data_source_file            c4qi00048j2.cif
_cod_data_source_block           eb1089
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4348218
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE O ( 25,X'S) H ( 252,X'S)
RIDE O ( 48,X'S) H ( 481,X'S)
RIDE O ( 65,X'S) H ( 650,X'S)
RIDE O ( 75,X'S) H ( 750,X'S)
RIDE O ( 77,X'S) H ( 770,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 27,X'S) H ( 271,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 29,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 301,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 33,X'S) H ( 331,X'S)
RIDE C ( 34,X'S) H ( 341,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 39,X'S) H ( 391,X'S)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 42,X'S) H ( 421,X'S)
RIDE C ( 43,X'S) H ( 431,X'S)
RIDE C ( 44,X'S) H ( 441,X'S)
RIDE C ( 45,X'S) H ( 451,X'S)
RIDE C ( 50,X'S) H ( 501,X'S)
RIDE C ( 51,X'S) H ( 511,X'S)
RIDE C ( 52,X'S) H ( 521,X'S)
RIDE C ( 53,X'S) H ( 531,X'S)
RIDE C ( 54,X'S) H ( 541,X'S)
RIDE C ( 56,X'S) H ( 561,X'S)
RIDE C ( 58,X'S) H ( 581,X'S)
RIDE C ( 59,X'S) H ( 591,X'S)
RIDE C ( 60,X'S) H ( 601,X'S)
RIDE C ( 61,X'S) H ( 611,X'S)
RIDE C ( 62,X'S) H ( 621,X'S)
RIDE C ( 67,X'S) H ( 671,X'S)
RIDE C ( 68,X'S) H ( 681,X'S)
RIDE C ( 69,X'S) H ( 691,X'S)
RIDE C ( 70,X'S) H ( 701,X'S)
RIDE C ( 71,X'S) H ( 711,X'S)
RIDE C ( 73,X'S) H ( 731,X'S) H ( 732,X'S)
RIDE C ( 76,X'S) H ( 761,X'S) H ( 762,X'S) H ( 763,X'S)
RIDE C ( 78,X'S) H ( 781,X'S) H ( 782,X'S) H ( 783,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
DIST 0.0, 0.01 = MEAN CL(1) TO C(73) , CL(2) TO C(73)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;