#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:59:16 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179909 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/05/7020503.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_7020503
loop_
_publ_author_name
'Armstrong, Jennifer A.'
'Williams, Edward R.'
'Weller, Mark T.'
_publ_section_title
;
 Cobalt(ii) fluorophosphate frameworks.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14180
_journal_page_last               14187
_journal_paper_doi               10.1039/c2dt31734f
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C4 H19.04 Co4 F N4 O17 P4'
_chemical_formula_weight         773.87
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-06-08 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8737(6)
_cell_length_b                   9.6815(4)
_cell_length_c                   13.6354(7)
_cell_measurement_reflns_used    3289
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1963.49(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8368
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    3.753
_exptl_absorpt_correction_T_max  0.9366
_exptl_absorpt_correction_T_min  0.9217
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0377P)²+13.7974P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                967
_reflns_number_total             1224
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2dt31734f_9.cif
_cod_data_source_block           2010jaa0049_cmcm
_cod_original_sg_symbol_H-M      Cmcm
_cod_database_code               7020503
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
OW1 O 0.0000 0.0829(10) 0.7500 0.042(2) Uani 1 4 d S
N2 N 0.1710(3) 0.0751(5) 0.6081(4) 0.0348(14) Uani 1 1 d .
H2A H 0.1741 0.1582 0.6357 0.052 Uiso 0.92 1 calc PR
H2B H 0.1845 0.0108 0.6523 0.052 Uiso 0.92 1 calc PR
H2C H 0.1155 0.0609 0.5858 0.052 Uiso 0.92 1 calc PR
C1 C 0.2649(4) 0.4326(6) 0.4740(5) 0.0376(16) Uani 1 1 d .
H1A H 0.2791 0.3603 0.5208 0.045 Uiso 1 1 calc R
H1B H 0.2049 0.4150 0.4492 0.045 Uiso 1 1 calc R
Co1 Co 0.12968(6) 0.70928(8) 0.7500 0.0097(3) Uani 1 2 d S
Co2 Co 0.0000 0.44880(9) 0.61241(7) 0.0119(3) Uani 1 2 d S
P3 P 0.0000 0.22600(17) 0.42674(13) 0.0120(4) Uani 1 2 d S
P4 P 0.16173(10) 0.38156(16) 0.7500 0.0093(4) Uani 1 2 d S
O1 O 0.1940(3) 0.5329(4) 0.7500 0.0122(10) Uani 1 2 d S
O2 O 0.1070(2) 0.3533(3) 0.6570(3) 0.0161(8) Uani 1 1 d .
O3 O 0.0000 0.6243(5) 0.5351(4) 0.0166(10) Uani 1 2 d S
O4 O 0.0855(2) 0.1960(3) 0.3686(3) 0.0174(8) Uani 1 1 d .
F1 F 0.0000 0.5822(5) 0.7500 0.0102(11) Uani 1 4 d S
F2 F 0.0000 0.1296(5) 0.5177(4) 0.0321(11) Uani 1 2 d S
O5 O 0.2430(3) 0.2874(4) 0.7500 0.0240(13) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
C1 N2 H2A 109.5 13_556 .
C1 N2 H2B 109.5 13_556 .
H2A N2 H2B 109.5 . .
C1 N2 H2C 109.5 13_556 .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
N2 C1 C1 114.0(5) 13_556 4_566
N2 C1 H1A 108.8 13_556 .
C1 C1 H1A 108.8 4_566 .
N2 C1 H1B 108.8 13_556 .
C1 C1 H1B 108.7 4_566 .
H1A C1 H1B 107.6 . .
O1 Co1 O4 124.66(10) . 11_566
O1 Co1 O4 124.66(10) . 4_566
O4 Co1 O4 110.2(2) 11_566 4_566
O1 Co1 O5 82.54(18) . 7_556
O4 Co1 O5 97.88(12) 11_566 7_556
O4 Co1 O5 97.88(12) 4_566 7_556
O1 Co1 F1 86.72(16) . .
O4 Co1 F1 88.21(11) 11_566 .
O4 Co1 F1 88.21(11) 4_566 .
O5 Co1 F1 169.26(17) 7_556 .
O2 Co2 O2 110.4(2) . 12
O2 Co2 O3 124.78(10) . .
O2 Co2 O3 124.78(10) 12 .
O2 Co2 O3 97.89(12) . 9_566
O2 Co2 O3 97.89(12) 12 9_566
O3 Co2 O3 77.6(2) . 9_566
O2 Co2 F1 90.71(12) . .
O2 Co2 F1 90.71(12) 12 .
O3 Co2 F1 87.25(17) . .
O3 Co2 F1 164.84(17) 9_566 .
O4 P3 O4 112.8(3) 12 .
O4 P3 O3 110.76(16) 12 9_566
O4 P3 O3 110.76(17) . 9_566
O4 P3 F2 107.52(17) 12 .
O4 P3 F2 107.52(17) . .
O3 P3 F2 107.2(3) 9_566 .
O5 P4 O2 108.49(16) . .
O5 P4 O2 108.49(16) . 10_557
O2 P4 O2 111.8(3) . 10_557
O5 P4 O1 108.9(3) . .
O2 P4 O1 109.57(16) . .
O2 P4 O1 109.57(16) 10_557 .
P4 O1 Co1 132.6(3) . .
P4 O2 Co2 127.7(2) . .
P3 O3 Co2 128.5(3) 9_566 .
P3 O3 Co2 129.1(3) 9_566 9_566
Co2 O3 Co2 102.4(2) . 9_566
P3 O4 Co1 128.0(2) . 11_565
Co2 F1 Co2 110.9(2) . 10_557
Co2 F1 Co1 107.754(16) . .
Co2 F1 Co1 107.754(16) 10_557 .
Co2 F1 Co1 107.754(16) . 3_556
Co2 F1 Co1 107.754(16) 10_557 3_556
Co1 F1 Co1 114.9(2) . 3_556
P4 O5 Co1 164.8(3) . 7_546
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N2 C1 1.473(8) 13_556
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
C1 N2 1.473(8) 13_556
C1 C1 1.485(13) 4_566
C1 H1A 0.9700 .
C1 H1B 0.9700 .
Co1 O1 1.958(4) .
Co1 O4 1.971(3) 11_566
Co1 O4 1.971(3) 4_566
Co1 O5 2.039(5) 7_556
Co1 F1 2.288(3) .
Co2 O2 1.938(3) .
Co2 O2 1.938(3) 12
Co2 O3 1.999(5) .
Co2 O3 2.133(5) 9_566
Co2 F1 2.278(3) .
P3 O4 1.526(3) 12
P3 O4 1.526(3) .
P3 O3 1.540(5) 9_566
P3 F2 1.552(5) .
P4 O5 1.514(5) .
P4 O2 1.532(3) .
P4 O2 1.532(3) 10_557
P4 O1 1.541(4) .
O3 P3 1.540(5) 9_566
O3 Co2 2.133(5) 9_566
O4 Co1 1.971(3) 11_565
F1 Co2 2.278(3) 10_557
F1 Co1 2.288(3) 3_556
O5 Co1 2.039(5) 7_546
