#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/57/2105724.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_2105724
loop_
_publ_author_name
'Munn, Alexis S.'
'Clarkson, Guy J.'
'Walton, Richard I.'
_publ_section_title
;
 Distortions of a flexible metal-organic framework from substituted
 pendant ligands
;
_journal_coeditor_code           BI5024
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              11
_journal_page_last               18
_journal_paper_doi               10.1107/S2052520613027224
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C14 H11 Co N O6'
_chemical_formula_sum            'C14 H11 Co N O6'
_chemical_formula_weight         348.17
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1507(2)
_cell_length_b                   18.1353(4)
_cell_length_c                   11.6447(3)
_cell_measurement_reflns_used    2929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.57
_cell_measurement_theta_min      3.79
_cell_volume                     1510.09(7)
_computing_cell_refinement       'CrysAlisRED, (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2006)'
_computing_data_reduction        CrysAlisRED
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7235
_diffrn_reflns_theta_full        70.68
_diffrn_reflns_theta_max         70.68
_diffrn_reflns_theta_min         4.51
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.182
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK (Oxford Diffraction, 2006)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.394
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1496
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0698P)²+3.5094P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1359
_reflns_number_gt                1426
_reflns_number_total             1496
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bi5024sup1.cif
_cod_data_source_block           Co-BDC-4-methyoxy-PNO
_cod_original_sg_symbol_Hall     '-p 2ac 2n'
_cod_database_code               2105724
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.22106(9) 0.7500 0.24179(5) 0.0103(2) Uani d S 1 2 . .
O O1 0.1264(4) 0.66666(16) 0.3479(3) 0.0389(7) Uani d U 1 1 . .
O O2 -0.1838(4) 0.66827(15) 0.3686(3) 0.0342(6) Uani d U 1 1 . .
C C2 -0.0250(5) 0.6408(2) 0.3801(4) 0.0342(7) Uani d U 1 1 . .
C C3 -0.0135(5) 0.5673(2) 0.4425(4) 0.0353(8) Uani d U 1 1 . .
C C4 0.1395(7) 0.5221(3) 0.4274(6) 0.0661(19) Uani d . 1 1 . .
H H4 0.2366 0.5367 0.3765 0.079 Uiso calc R 1 1 . .
C C5 -0.1530(7) 0.5442(3) 0.5145(6) 0.0666(19) Uani d . 1 1 . .
H H5 -0.2607 0.5742 0.5247 0.080 Uiso calc R 1 1 . .
O O6 -0.0343(4) 0.7500 0.1599(3) 0.0193(7) Uani d SD 1 2 . .
N N7 -0.0485(5) 0.7414(2) 0.0481(3) 0.0255(14) Uani d PGD 0.50 1 A -1
C C8 -0.0432(9) 0.8029(2) -0.0233(3) 0.033(3) Uani d PG 0.50 1 A -1
H H8 -0.0297 0.8507 0.0088 0.039 Uiso calc PR 0.50 1 A -1
C C9 -0.0578(9) 0.7942(2) -0.1415(3) 0.029(2) Uani d PG 0.50 1 A -1
H H9 -0.0542 0.8362 -0.1903 0.035 Uiso calc PR 0.50 1 A -1
C C10 -0.0776(7) 0.7242(3) -0.1885(3) 0.029(2) Uani d PGD 0.50 1 A -1
C C11 -0.0828(10) 0.6628(2) -0.1172(3) 0.0309(18) Uani d PG 0.50 1 A -1
H H11 -0.0963 0.6149 -0.1493 0.037 Uiso calc PR 0.50 1 A -1
C C12 -0.0683(9) 0.6714(2) 0.0011(3) 0.029(2) Uani d PG 0.50 1 A -1
H H12 -0.0719 0.6294 0.0498 0.035 Uiso calc PR 0.50 1 A -1
O O13 -0.0922(9) 0.7116(4) -0.3012(5) 0.0444(15) Uani d PD 0.50 1 A -1
C C14 -0.0802(12) 0.7739(5) -0.3774(7) 0.046(3) Uani d PD 0.50 1 A -1
H H14A -0.0996 0.7575 -0.4567 0.069 Uiso calc PR 0.50 1 A -1
H H14B 0.0436 0.7966 -0.3705 0.069 Uiso calc PR 0.50 1 A -1
H H14C -0.1765 0.8100 -0.3569 0.069 Uiso calc PR 0.50 1 A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O6 Co1 O1 . 7_575 89.23(10)
O6 Co1 O1 . . 89.23(10)
O1 Co1 O1 7_575 . 94.0(2)
O6 Co1 O2 . 4_565 90.22(10)
O1 Co1 O2 7_575 4_565 87.44(13)
O1 Co1 O2 . 4_565 178.43(14)
O6 Co1 O2 . 6_656 90.22(10)
O1 Co1 O2 7_575 6_656 178.43(14)
O1 Co1 O2 . 6_656 87.44(13)
O2 Co1 O2 4_565 6_656 91.09(19)
O6 Co1 O6 . 6_656 174.38(9)
O1 Co1 O6 7_575 6_656 86.93(10)
O1 Co1 O6 . 6_656 86.93(10)
O2 Co1 O6 4_565 6_656 93.71(10)
O2 Co1 O6 6_656 6_656 93.71(10)
C2 O1 Co1 . . 138.1(2)
C2 O2 Co1 . 6_556 130.6(2)
O1 C2 O2 . . 127.7(3)
O1 C2 C3 . . 115.5(3)
O2 C2 C3 . . 116.8(3)
C5 C3 C4 . . 118.3(4)
C5 C3 C2 . . 121.5(4)
C4 C3 C2 . . 120.2(4)
C3 C4 C5 . 5_566 120.6(4)
C3 C4 H4 . . 119.7
C5 C4 H4 5_566 . 119.7
C3 C5 C4 . 5_566 121.0(4)
C3 C5 H5 . . 119.5
C4 C5 H5 5_566 . 119.5
N7 O6 Co1 7_575 . 121.8(3)
N7 O6 Co1 . . 121.8(3)
N7 O6 Co1 7_575 6_556 118.5(3)
N7 O6 Co1 . 6_556 118.5(3)
Co1 O6 Co1 . 6_556 119.22(15)
O6 N7 C8 . . 119.7(2)
O6 N7 C12 . . 120.4(2)
C8 N7 C12 . . 120.0
N7 C8 C9 . . 120.0
N7 C8 H8 . . 120.0
C9 C8 H8 . . 120.0
C8 C9 C10 . . 120.0
C8 C9 H9 . . 120.0
C10 C9 H9 . . 120.0
O13 C10 C11 . . 116.6(4)
O13 C10 C9 . . 123.4(4)
C11 C10 C9 . . 120.0
C10 C11 C12 . . 120.0
C10 C11 H11 . . 120.0
C12 C11 H11 . . 120.0
C11 C12 N7 . . 120.0
C11 C12 H12 . . 120.0
N7 C12 H12 . . 120.0
C10 O13 C14 . . 117.8(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O6 . 2.060(3)
Co1 O1 7_575 2.066(2)
Co1 O1 . 2.066(2)
Co1 O2 4_565 2.077(2)
Co1 O2 6_656 2.077(2)
Co1 O6 6_656 2.091(3)
O1 C2 . 1.239(5)
O2 C2 . 1.247(5)
O2 Co1 6_556 2.077(2)
C2 C3 . 1.519(5)
C3 C5 . 1.369(6)
C3 C4 . 1.379(7)
C4 C5 5_566 1.384(6)
C4 H4 . 0.9500
C5 C4 5_566 1.384(6)
C5 H5 . 0.9500
O6 N7 7_575 1.315(4)
O6 N7 . 1.315(4)
O6 Co1 6_556 2.091(3)
N7 C8 . 1.3900
N7 C12 . 1.3900
C8 C9 . 1.3900
C8 H8 . 0.9500
C9 C10 . 1.3900
C9 H9 . 0.9500
C10 O13 . 1.337(7)
C10 C11 . 1.3900
C11 C12 . 1.3900
C11 H11 . 0.9500
C12 H12 . 0.9500
O13 C14 . 1.439(10)
C14 H14A . 0.9800
C14 H14B . 0.9800
C14 H14C . 0.9800
