#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/34/4323495.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4323495
loop_
_publ_author_name
'Hiroki Oshio'
'Hiroshi Okamoto'
'Toshihiko Kikuchi'
'Tasuku Ito'
_publ_contact_author
;
     Hiroki OSHIO name
     Departmento of Chemistry, Graduate School of Science
     Tohoku University
     Sendai 980-77
     Japan
;
_publ_contact_author_email       oshio@agnus.chem.tohoku.ac.jp
_publ_contact_author_fax         +81-22-217-6548
_publ_contact_author_phone       +81-22-217-6545
_publ_section_title
;
 The Ferromagnetic Chain System catena-(μ-CrO4-O,O')[NiII(cyclam)].2H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3201
_journal_page_last               3203
_journal_paper_doi               10.1021/ic970180m
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C10 H28 Cr N4 Ni O6'
_chemical_formula_weight         411.05
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   fdif
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   fdif
_audit_creation_date             95-04-28
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                92.86(2)
_cell_angle_beta                 117.74(2)
_cell_angle_gamma                105.06(2)
_cell_formula_units_Z            2
_cell_length_a                   9.156(2)
_cell_length_b                   12.168(2)
_cell_length_c                   9.027(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    213
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      12.5
_cell_volume                     842.2(4)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        xtal_DIFDAT_ADDREF_SORTRF
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    xtal
_diffrn_ambient_temperature      213.15
_diffrn_measurement_device       Rigaku5
_diffrn_measurement_method       '2θ/ω sans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           xray_tube
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .011
_diffrn_reflns_av_sigmaI/netI    .019
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4102
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.77
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    18.2
_exptl_absorpt_correction_T_max  1.06
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       tablet
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.50
_refine_diff_density_max         .491
_refine_diff_density_min         -.838
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.593
_refine_ls_goodness_of_fit_obs   1.652
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     314
_refine_ls_number_reflns         3444
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .031
_refine_ls_R_factor_obs          .027
_refine_ls_shift/esd_max         1.397
_refine_ls_shift/esd_mean        .165
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .037
_refine_ls_wR_factor_obs         .036
_reflns_d_resolution_high        .77
_reflns_d_resolution_low         11.487
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              10
_reflns_limit_l_min              -11
_reflns_number_observed          3444
_reflns_number_total             3858
_reflns_observed_criterion       >3sigma(I)
_cod_data_source_file            ic970180m.cif
_cod_data_source_block           nicro4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '-60' was changed to '213.15' -
it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Heavy atom method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_Hall     -P_1
_cod_database_code               4323495
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni1 .0134(2) .0104(2) .0148(2) .0036(1) .0074(1) .0022(1)
Ni2 .0161(2) .0096(2) .0200(2) .0030(1) .0113(1) .0023(1)
Cr .0161(2) .0102(1) .0212(2) .0021(1) .0117(1) .0027(1)
O1 .0249(7) .0111(6) .0253(7) .0021(5) .0153(6) .0028(5)
O2 .0222(7) .0156(7) .0289(8) .0019(6) .0153(6) .0059(6)
O3 .0311(8) .0234(8) .049(1) .0117(7) .0295(8) .0092(7)
O4 .0269(8) .0244(8) .0227(7) -.0001(6) .0097(6) .0028(6)
O5 .035(1) .033(1) .038(1) .0102(8) .0137(8) .0027(8)
O6 .065(2) .043(1) .053(1) .018(1) .002(1) .001(1)
N1 .0193(8) .0140(8) .0175(8) .0035(7) .0096(7) .0035(6)
N2 .0167(8) .0131(8) .0236(8) .0049(6) .0109(7) .0042(6)
N3 .030(1) .0171(9) .045(1) .0020(7) .0274(9) -.0036(8)
N4 .0174(9) .028(1) .032(1) .0043(7) .0134(8) .0138(8)
C1 .022(1) .027(1) .021(1) .0108(9) .0068(9) .0073(8)
C2 .029(1) .023(1) .018(1) .0068(9) .0144(9) .0045(8)
C3 .033(1) .021(1) .028(1) .0075(9) .021(1) .0028(8)
C4 .022(1) .020(1) .031(1) .0070(8) .0184(9) .0051(8)
C5 .0163(9) .028(1) .028(1) .0092(8) .0077(8) .0034(9)
C6 .024(1) .054(2) .027(1) -.003(1) .008(1) .011(1)
C7 .042(2) .064(2) .025(1) -.014(1) .017(1) -.012(1)
C8 .044(2) .033(1) .052(2) -.009(1) .031(1) -.022(1)
C9 .046(2) .019(1) .080(2) .017(1) .043(2) .012(1)
C10 .032(1) .039(1) .067(2) .023(1) .029(1) .029(1)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Ni1 .00000 .00000 1.00000 .0128(1) Uani ? ?
Ni2 .50000 .50000 1.00000 .0146(1) Uani ? ?
Cr .18907(4) .29116(2) 1.05547(4) .0152(1) Uani ? ?
O1 .1162(2) .1556(1) .9515(2) .0201(5) Uani ? ?
O2 .2702(2) .3808(1) .9620(2) .0220(5) Uani ? ?
O3 .0267(2) .3243(1) 1.0602(2) .0294(6) Uani ? ?
O4 .3429(2) .3004(1) 1.2511(2) .0276(5) Uani ? ?
O5 -.1616(3) .4292(2) .7908(3) .0380(7) Uani ? ?
O6 .6419(4) .2454(2) .4946(3) .066(1) Uani ? ?
N1 -.1534(2) -.0592(1) .7385(2) .0171(6) Uani ? ?
N2 .1970(2) -.0638(1) 1.0213(2) .0173(6) Uani ? ?
N3 .5335(3) .3766(2) .8645(3) .0283(7) Uani ? ?
N4 .3543(2) .5597(2) .7876(3) .0260(7) Uani ? ?
C1 -.2830(3) .0031(2) .6805(3) .0245(8) Uani ? ?
C2 -.0573(3) -.0485(2) .6438(3) .0227(7) Uani ? ?
C3 .0780(3) -.1113(2) .7082(3) .0252(8) Uani ? ?
C4 .2382(3) -.0520(2) .8824(3) .0223(7) Uani ? ?
C5 .3474(3) -.0067(2) 1.1924(3) .0249(8) Uani ? ?
C6 .2297(3) .4720(3) .6310(3) .041(1) Uani ? ?
C7 .3189(4) .4009(3) .5819(4) .051(1) Uani ? ?
C8 .3794(4) .3165(2) .6949(4) .045(1) Uani ? ?
C9 .5952(4) .2980(2) .9807(4) .042(1) Uani ? ?
C10 .2742(4) .6319(2) .8429(4) .041(1) Uani ? ?
H1n -.207(3) -.128(2) .725(3) .016(6) Uiso ? ?
H2n .163(3) -.132(2) 1.026(3) .026(7) Uiso ? ?
H3n .617(3) .410(2) .849(3) .022(6) Uiso ? ?
H4n .417(4) .594(3) .769(4) .035(8) Uiso ? ?
H1a -.373(3) -.032(2) .570(3) .025(6) Uiso ? ?
H1b -.230(3) .079(2) .684(3) .030(7) Uiso ? ?
H2a -.132(3) -.077(2) .528(3) .021(6) Uiso ? ?
H2b -.004(3) .035(2) .652(3) .014(5) Uiso ? ?
H3a .029(3) -.187(2) .711(3) .021(6) Uiso ? ?
H3b .117(4) -.121(2) .620(3) .037(7) Uiso ? ?
H4a .331(3) -.082(2) .902(3) .028(7) Uiso ? ?
H4b .288(3) .030(2) .885(3) .023(6) Uiso ? ?
H5a .406(3) .079(2) 1.188(3) .018(6) Uiso ? ?
H5b .436(4) -.043(2) 1.232(3) .033(7) Uiso ? ?
H6a .146(4) .426(3) .652(4) .041(8) Uiso ? ?
H6b .162(4) .515(3) .537(5) .07(1) Uiso ? ?
H7a .427(4) .452(3) .583(4) .051(9) Uiso ? ?
H7b .246(4) .361(3) .480(4) .06(1) Uiso ? ?
H8a .290(4) .273(2) .715(3) .034(7) Uiso ? ?
H8b .412(5) .264(3) .643(5) .07(1) Uiso ? ?
H9a .499(4) .251(3) .978(4) .041(8) Uiso ? ?
H9b .643(4) .244(3) .938(4) .055(9) Uiso ? ?
H10a .180(4) .579(3) .851(4) .038(7) Uiso ? ?
H10b .232(4) .684(3) .769(4) .06(1) Uiso ? ?
H11a .552(5) .266(3) .434(5) .06(1) Uiso ? ?
H11b .724(5) .303(3) .585(5) .07(1) Uiso ? ?
H12a -.089(4) .403(3) .881(4) .044(8) Uiso ? ?
H12b -.108(4) .503(3) .828(4) .06(1) Uiso ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni ? 0 2 .285 1.113 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
Cr ? 0 2 .284 .624 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
O ? 0 12 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
N ? 0 8 .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
C ? 0 20 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
H ? 0 56 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
