#------------------------------------------------------------------------------
#$Date: 2019-11-23 23:48:53 +0200 (Sat, 23 Nov 2019) $
#$Revision: 235651 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/21/7702149.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_7702149
loop_
_publ_author_name
'Escobedo-Cruz, Francisco V'
'Hughbanks, Timothy'
_publ_section_title
;
 New coordination networks containing trinuclear lanthanide complexes and
 hexacyanometallates.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6831
_journal_page_last               6841
_journal_paper_doi               10.1039/c7dt02541f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C30 H56 Cr Gd3 N12 O10'
_chemical_formula_sum            'C30 H56 Cr Gd3 N12 O10'
_chemical_formula_weight         1268.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.419(6)
_cell_length_b                   13.366(6)
_cell_length_c                   13.772(6)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.23
_cell_measurement_theta_min      2.55
_cell_volume                     2654(2)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25425
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.054
_diffrn_reflns_theta_min         2.045
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.950
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1396 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.6079.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       needle
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.989
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0167
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0202P)²+1.3095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2365
_reflns_number_total             2533
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02541f1.cif
_cod_data_source_block           C30H56N12O10Gd3Cr
_cod_original_cell_volume        2654.2(19)
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               7702149
_shelxl_version_number           2014-1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H4d(0.5) H4e(0.5) H1a(0.5) H1b(0.5)
3.a Rotating group:
 O4(H4d,H4e), O1(H1a,H1b)
3.b Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9)
3.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C7(H7a,H7b,H7c), C10(H10a,H10b,H10c)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Gd2 Gd 0.2500 0.2500 0.95622(2) 0.02464(7) Uani 1 4 d S T P
Gd1 Gd 0.2500 0.11416(2) 0.72205(2) 0.01837(6) Uani 1 2 d S T P
Cr1 Cr 0.2500 -0.2500 0.54971(6) 0.0337(2) Uani 1 4 d S T P
O3 O 0.16323(11) 0.13981(12) 0.86315(12) 0.0265(4) Uani 1 1 d . . .
O2 O 0.33785(16) 0.2500 0.68124(16) 0.0246(5) Uani 1 2 d S T P
N1 N 0.2500 -0.0695(2) 0.7054(2) 0.0357(7) Uani 1 2 d S T P
C1 C 0.2500 -0.1378(3) 0.6532(3) 0.0330(8) Uani 1 2 d S T P
N4 N 0.07420(15) 0.06567(15) 0.70014(15) 0.0309(5) Uani 1 1 d . . .
N5 N 0.0738(2) 0.2500 1.0077(2) 0.0424(8) Uani 1 2 d S T P
C5 C 0.4345(2) 0.2500 0.6958(3) 0.0286(8) Uani 1 2 d S T P
H5 H 0.4643 0.2500 0.6318 0.034 Uiso 1 2 calc RS T P
C6 C 0.46504(17) 0.15536(19) 0.7492(2) 0.0315(6) Uani 1 1 d . . .
H6 H 0.5329 0.1512 0.7471 0.038 Uiso 1 1 calc R . .
C8 C 0.06607(17) 0.15470(19) 0.85537(18) 0.0303(6) Uani 1 1 d . . .
H8 H 0.0354 0.0982 0.8874 0.036 Uiso 1 1 calc R . .
C9 C 0.0357(3) 0.2500 0.9074(3) 0.0354(9) Uani 1 2 d S T P
H9 H -0.0321 0.2500 0.9116 0.042 Uiso 1 2 calc RS T P
C2 C 0.1064(3) -0.2500 0.5559(3) 0.0403(10) Uani 1 2 d S T P
N2 N 0.0278(3) -0.2500 0.5649(3) 0.0475(9) Uani 1 2 d S T P
C4 C 0.0415(2) 0.0586(2) 0.5988(2) 0.0453(7) Uani 1 1 d . . .
H4A H 0.0623 0.1161 0.5631 0.068 Uiso 1 1 calc GR . .
H4B H -0.0250 0.0562 0.5979 0.068 Uiso 1 1 calc GR . .
H4C H 0.0660 -0.0010 0.5695 0.068 Uiso 1 1 calc GR . .
C7 C 0.0432(2) -0.0268(2) 0.7495(2) 0.0400(7) Uani 1 1 d . . .
H7A H 0.0585 -0.0837 0.7101 0.060 Uiso 1 1 calc GR . .
H7B H -0.0227 -0.0243 0.7591 0.060 Uiso 1 1 calc GR . .
H7C H 0.0737 -0.0323 0.8112 0.060 Uiso 1 1 calc GR . .
C10 C 0.0420(2) 0.3393(3) 1.0620(2) 0.0636(10) Uani 1 1 d . . .
H10A H 0.0604 0.3336 1.1288 0.095 Uiso 1 1 calc GR . .
H10B H -0.0244 0.3440 1.0582 0.095 Uiso 1 1 calc GR . .
H10C H 0.0692 0.3983 1.0343 0.095 Uiso 1 1 calc GR . .
O4 O 0.2500 0.1304(3) 1.0851(2) 0.0616(9) Uani 1 2 d S T P
H4D H 0.2713 0.1399 1.1533 0.092 Uiso 0.5 1 d GR . .
H4E H 0.2284 0.0595 1.0831 0.092 Uiso 0.5 1 d GR . .
O1 O 0.2500 0.09463(19) 0.54725(17) 0.0417(7) Uani 1 2 d S T P
H1A H 0.2049 0.1325 0.5172 0.063 Uiso 0.5 1 d GR . .
H1B H 0.2337 0.0310 0.5278 0.063 Uiso 0.5 1 d GR . .
C3 C 0.2500 -0.1372(3) 0.4451(3) 0.0411(10) Uani 1 2 d S T P
N3 N 0.2500 -0.0704(3) 0.3924(3) 0.0529(10) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Gd1 Gd2 Gd1 58.76(3) . 2
O3 Gd2 Gd1 37.51(4) 7_655 .
O3 Gd2 Gd1 37.51(4) 8_565 2
O3 Gd2 Gd1 37.51(4) . .
O3 Gd2 Gd1 80.21(5) 7_655 2
O3 Gd2 Gd1 80.21(5) 2 .
O3 Gd2 Gd1 37.51(4) 2 2
O3 Gd2 Gd1 80.21(5) 8_565 .
O3 Gd2 Gd1 80.21(5) . 2
O3 Gd2 O3 78.86(9) 7_655 2
O3 Gd2 O3 78.86(9) 8_565 .
O3 Gd2 O3 112.90(8) 7_655 8_565
O3 Gd2 O3 65.31(8) 7_655 .
O3 Gd2 O3 112.90(8) 2 .
O3 Gd2 O3 65.31(8) 2 8_565
O3 Gd2 N5 68.21(7) 2 2
O3 Gd2 N5 131.93(6) 8_565 2
O3 Gd2 N5 131.93(6) 2 .
O3 Gd2 N5 68.21(7) . .
O3 Gd2 N5 68.21(7) 8_565 .
O3 Gd2 N5 131.93(6) 7_655 .
O3 Gd2 N5 68.21(7) 7_655 2
O3 Gd2 N5 131.93(6) . 2
O3 Gd2 O4 89.18(9) 2 2
O3 Gd2 O4 146.69(4) 7_655 2
O3 Gd2 O4 146.69(4) . 2
O3 Gd2 O4 146.69(4) 8_565 .
O3 Gd2 O4 89.18(9) 8_565 2
O3 Gd2 O4 89.18(9) 7_655 .
O3 Gd2 O4 146.69(4) 2 .
O3 Gd2 O4 89.18(9) . .
N5 Gd2 Gd1 103.54(6) 2 .
N5 Gd2 Gd1 103.54(6) 2 2
N5 Gd2 Gd1 103.54(6) . .
N5 Gd2 Gd1 103.54(6) . 2
N5 Gd2 N5 148.82(14) . 2
O4 Gd2 Gd1 167.38(8) 2 .
O4 Gd2 Gd1 167.38(8) . 2
O4 Gd2 Gd1 108.62(9) . .
O4 Gd2 Gd1 108.62(9) 2 2
O4 Gd2 N5 78.48(6) 2 .
O4 Gd2 N5 78.48(6) 2 2
O4 Gd2 N5 78.48(6) . .
O4 Gd2 N5 78.48(6) . 2
O4 Gd2 O4 84.01(17) 2 .
Gd1 Gd1 Gd2 60.621(15) 2 .
O3 Gd1 Gd2 37.18(4) 7_655 .
O3 Gd1 Gd2 37.18(4) . .
O3 Gd1 Gd1 81.56(4) 7_655 2
O3 Gd1 Gd1 81.56(4) . 2
O3 Gd1 O3 64.75(8) . 7_655
O3 Gd1 N1 102.92(7) . .
O3 Gd1 N1 102.92(7) 7_655 .
O3 Gd1 N4 130.30(6) . 7_655
O3 Gd1 N4 130.30(6) 7_655 .
O3 Gd1 N4 67.42(6) . .
O3 Gd1 N4 67.42(6) 7_655 7_655
O3 Gd1 O1 147.42(4) . .
O3 Gd1 O1 147.42(4) 7_655 .
O2 Gd1 Gd2 79.88(6) 2 .
O2 Gd1 Gd2 79.89(6) . .
O2 Gd1 Gd1 37.35(5) . 2
O2 Gd1 Gd1 37.35(5) 2 2
O2 Gd1 O3 77.94(7) . 7_655
O2 Gd1 O3 112.64(7) . .
O2 Gd1 O3 77.93(7) 2 .
O2 Gd1 O3 112.64(7) 2 7_655
O2 Gd1 O2 67.37(10) 2 .
O2 Gd1 N1 140.22(6) . .
O2 Gd1 N1 140.22(6) 2 .
O2 Gd1 N4 68.51(7) . 7_655
O2 Gd1 N4 134.52(7) . .
O2 Gd1 N4 134.52(7) 2 7_655
O2 Gd1 N4 68.51(7) 2 .
O2 Gd1 O1 80.86(7) 2 .
O2 Gd1 O1 80.86(7) . .
N1 Gd1 Gd2 124.73(8) . .
N1 Gd1 Gd1 174.65(7) . 2
N1 Gd1 N4 75.19(5) . 7_655
N1 Gd1 N4 75.19(5) . .
N4 Gd1 Gd2 102.74(5) . .
N4 Gd1 Gd2 102.74(5) 7_655 .
N4 Gd1 Gd1 104.24(5) . 2
N4 Gd1 Gd1 104.24(5) 7_655 2
N4 Gd1 N4 148.50(9) . 7_655
O1 Gd1 Gd2 156.81(6) . .
O1 Gd1 Gd1 96.19(6) . 2
O1 Gd1 N1 78.47(9) . .
O1 Gd1 N4 81.93(5) . .
O1 Gd1 N4 81.93(5) . 7_655
C1 Cr1 C1 92.9(2) . 2_545
C1 Cr1 C2 88.38(8) 2_545 .
C1 Cr1 C2 88.38(8) . .
C1 Cr1 C2 88.38(8) . 2_545
C1 Cr1 C2 88.38(8) 2_545 2_545
C1 Cr1 C3 179.84(15) 2_545 .
C1 Cr1 C3 87.23(15) 2_545 2_545
C1 Cr1 C3 87.23(15) . .
C1 Cr1 C3 179.84(15) . 2_545
C2 Cr1 C2 175.3(2) . 2_545
C2 Cr1 C3 91.63(8) 2_545 .
C2 Cr1 C3 91.63(8) . .
C2 Cr1 C3 91.63(8) 2_545 2_545
C2 Cr1 C3 91.63(8) . 2_545
C3 Cr1 C3 92.6(2) . 2_545
Gd2 O3 Gd1 105.30(7) . .
C8 O3 Gd2 119.04(14) . .
C8 O3 Gd1 119.10(14) . .
Gd1 O2 Gd1 105.30(9) . 2
C5 O2 Gd1 120.93(9) . .
C5 O2 Gd1 120.93(9) . 2
C1 N1 Gd1 147.1(3) . .
N1 C1 Cr1 174.7(3) . .
C6 N4 Gd1 96.65(14) 7_655 .
C4 N4 Gd1 115.55(17) . .
C4 N4 C6 111.1(2) . 7_655
C4 N4 C7 106.5(2) . .
C7 N4 Gd1 116.33(16) . .
C7 N4 C6 110.5(2) . 7_655
C9 N5 Gd2 96.1(2) . .
C10 N5 Gd2 115.7(2) . .
C10 N5 Gd2 115.7(2) 8_565 .
C10 N5 C9 110.8(2) . .
C10 N5 C9 110.8(2) 8_565 .
C10 N5 C10 107.3(4) 8_565 .
O2 C5 C6 110.72(18) . .
O2 C5 C6 110.72(18) . 8_565
C6 C5 C6 111.7(3) . 8_565
N4 C6 C5 109.8(2) 7_655 .
N4 C6 C8 108.5(2) 7_655 7_655
C5 C6 C8 112.4(2) . 7_655
O3 C8 C6 111.3(2) . 7_655
O3 C8 C9 111.4(2) . .
C9 C8 C6 111.1(2) . 7_655
N5 C9 C8 109.3(2) . 8_565
N5 C9 C8 109.3(2) . .
C8 C9 C8 113.2(3) 8_565 .
N2 C2 Cr1 176.1(4) . .
N3 C3 Cr1 175.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd2 Gd1 3.7010(13) .
Gd2 Gd1 3.7010(13) 2
Gd2 O3 2.3189(17) 8_565
Gd2 O3 2.3189(17) 2
Gd2 O3 2.3189(17) .
Gd2 O3 2.3189(17) 7_655
Gd2 N5 2.637(4) 2
Gd2 N5 2.637(4) .
Gd2 O4 2.389(3) .
Gd2 O4 2.389(3) 2
Gd1 Gd1 3.6314(15) 2
Gd1 O3 2.3366(17) 7_655
Gd1 O3 2.3366(17) .
Gd1 O2 2.2842(15) .
Gd1 O2 2.2841(15) 2
Gd1 N1 2.465(3) .
Gd1 N4 2.634(2) .
Gd1 N4 2.634(2) 7_655
Gd1 O1 2.421(3) .
Cr1 C1 2.069(4) 2_545
Cr1 C1 2.069(4) .
Cr1 C2 2.072(5) 2_545
Cr1 C2 2.072(5) .
Cr1 C3 2.086(4) .
Cr1 C3 2.086(4) 2_545
O3 C8 1.419(3) .
O2 Gd1 2.2842(15) 2
O2 C5 1.408(4) .
N1 C1 1.162(5) .
N4 C6 1.488(4) 7_655
N4 C4 1.476(3) .
N4 C7 1.479(3) .
N5 C9 1.487(5) .
N5 C10 1.482(4) 8_565
N5 C10 1.482(4) .
C5 C6 1.528(3) .
C5 C6 1.528(3) 8_565
C6 N4 1.488(4) 7_655
C6 C8 1.530(4) 7_655
C8 C6 1.530(4) 7_655
C8 C9 1.525(3) .
C9 C8 1.525(3) 8_565
C2 N2 1.141(5) .
C3 N3 1.151(5) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1B N3 0.92 2.32 3.068(5) 138.4
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.002 -0.041 0.000 754.5 194.3 '20 H2O'
