#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/44/2014424.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2014424
loop_
_publ_author_name
'Boča, Miroslav'
'Ingrid Svoboda'
'Franz Renz'
'Hartmut Fuess'
_publ_section_title
;
 Poly[methylammonium
 tris(μ₂-formato-κ²O:O')cobalt(II)]
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m631
_journal_page_last               m633
_journal_paper_doi               10.1107/S0108270104025776
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C H6 N) [Co (C O2)3]'
_chemical_formula_moiety         'C H6 N1 +, C3 H3 Co O6 -'
_chemical_formula_sum            'C4 H9 Co N O6'
_chemical_formula_weight         226.05
_chemical_name_systematic
;
Poly[methylammonium [tris(μ₂-formato-κ²O:O')cobalt(II)]]
;
_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                   8.4069(9)
_cell_length_b                   11.7100(10)
_cell_length_c                   8.1075(9)
_cell_measurement_reflns_used    899
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      23.11
_cell_measurement_theta_min      3.69
_cell_volume                     798.14(14)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2001)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2001)
;
_computing_data_reduction
;
CrysAlis RED
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003)
;
_computing_publication_material  reference?
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 'Sapphire CCD detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method
;
Rotation method data acquisition using ω
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5931
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.143
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.622
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1173
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0494
_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)+(0.1P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1595
_reflns_number_gt                854
_reflns_number_total             1173
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            av1205.cif
_cod_data_source_block           I
_cod_database_code               2014424
_cod_database_fobs_code          2014424
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
C1 0.2788(5) 0.5293(4) 0.2195(5) 0.0261(8) Uani d . 1 . . C
H1 0.235(5) 0.463(4) 0.272(5) 0.031 Uiso d . 1 . . H
C2 0.0122(6) 0.2500 0.0550(8) 0.0240(11) Uani d S 1 . . C
H2 -0.009(6) 0.2500 -0.064(9) 0.029 Uiso d S 1 . . H
C3 0.4218(10) 0.2500 -0.0204(9) 0.0507(19) Uani d SD 1 . . C
H3A 0.3710(17) 0.1870(4) 0.022(2) 0.061 Uiso d D 1 . . H
H3B 0.413(3) 0.2500 -0.1329(15) 0.061 Uiso d SD 1 . . H
O1 0.2231(3) 0.5606(2) 0.0834(3) 0.0256(6) Uani d . 1 . . O
O2 0.4025(3) 0.5676(2) 0.2835(3) 0.0287(6) Uani d . 1 . . O
O3 0.0283(3) 0.3440(2) 0.1260(3) 0.0277(6) Uani d . 1 . . O
N4 0.5835(7) 0.2500 0.0277(6) 0.0339(12) Uani d SD 1 . . N
H4A 0.636(5) 0.187(3) 0.001(5) 0.041 Uiso d D 1 . . H
H4B 0.593(7) 0.2500 0.1368(17) 0.041 Uiso d SD 1 . . H
Co1 0.0000 0.5000 0.0000 0.0179(3) Uani d S 1 . . Co
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
C1 0.0262(18) 0.0253(17) 0.0268(19) -0.0031(15) -0.0010(16) 0.0021(16)
C2 0.023(3) 0.027(3) 0.022(3) 0.000 -0.0028(19) 0.000
C3 0.045(5) 0.058(5) 0.049(4) 0.000 0.001(3) 0.000
O1 0.0252(12) 0.0311(14) 0.0205(12) -0.0029(11) -0.0062(10) 0.0034(11)
O2 0.0288(13) 0.0316(14) 0.0258(13) -0.0058(11) -0.0088(11) 0.0063(12)
O3 0.0400(15) 0.0184(13) 0.0246(13) -0.0019(11) -0.0043(11) 0.0010(11)
N4 0.039(3) 0.034(3) 0.029(3) 0.000 0.012(2) 0.000
Co1 0.0190(4) 0.0182(4) 0.0165(4) -0.0019(2) 0.0002(2) 0.0001(2)
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'
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'
Co Co 0.3494 0.9721 '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
_geom_angle_publ_flag
O2 C1 O1 . . 125.0(4) yes
O2 C1 H1 . . 116(2) ?
O1 C1 H1 . . 119(2) ?
O3 C2 O3 . 8_565 123.5(6) yes
O3 C2 H2 . . 118.2(3) ?
N4 C3 H3A . . 110.0(12) ?
N4 C3 H3B . . 110.9(18) ?
H3A C3 H3B . . 109.6(12) ?
C1 O1 Co1 . . 121.0(2) ?
C1 O2 Co1 . 2_565 122.7(3) ?
C2 O3 Co1 . . 121.9(3) ?
C3 N4 H4A . . 114(3) ?
C3 N4 H4B . . 111(4) ?
H4A N4 H4B . . 101(4) ?
O2 Co1 O2 6_556 2_564 180.0 yes
O2 Co1 O3 6_556 . 88.03(10) ?
O2 Co1 O3 2_564 . 91.97(10) ?
O3 Co1 O3 . 5_565 180.00(7) yes
O2 Co1 O1 6_556 . 87.27(10) ?
O2 Co1 O1 2_564 . 92.73(10) ?
O3 Co1 O1 . . 92.07(10) yes
O3 Co1 O1 5_565 . 87.93(10) ?
O2 Co1 O1 6_556 5_565 92.73(10) ?
O1 Co1 O1 . 5_565 180.0 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O2 . 1.245(4) yes
C1 O1 . 1.253(4) yes
C1 H1 . 0.95(5) ?
C2 O3 . 1.249(4) yes
C2 H2 . 0.98(8) ?
C3 N4 . 1.414(11) yes
C3 H3A . 0.920(6) ?
C3 H3B . 0.915(10) ?
O1 Co1 . 2.117(2) yes
O2 Co1 2_565 2.093(2) yes
O3 Co1 . 2.107(2) yes
N4 H4A . 0.890(10) ?
N4 H4B . 0.890(10) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N4 H4A O1 4_645 0.890(10) 2.010(10) 2.893(4) 170(5) yes
N4 H4B O3 6_656 0.890(10) 2.28(2) 3.051(5) 145(3) yes
N4 H4B O3 3 0.890(10) 2.28(2) 3.051(5) 145(3) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O2 C1 O1 Co1 . . -174.0(3)
O1 C1 O2 Co1 . 2_565 -173.9(3)
O3 C2 O3 Co1 8_565 . 180.0(3)
C2 O3 Co1 O2 . 6_556 145.1(3)
C2 O3 Co1 O2 . 2_564 -34.9(3)
C2 O3 Co1 O1 . . -127.7(3)
C2 O3 Co1 O1 . 5_565 52.3(3)
C1 O1 Co1 O2 . 6_556 57.8(3)
C1 O1 Co1 O2 . 2_564 -122.2(3)
C1 O1 Co1 O3 . . -30.2(3)
C1 O1 Co1 O3 . 5_565 149.8(3)
