#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/29/7012933.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_7012933
loop_
_publ_author_name
'Barnett, Sarah A.'
'Blake, Alexander J.'
'Champness, Neil R.'
'Wilson, Claire'
_publ_section_title
;
 The r�le of 4,7-phenanthroline in coordination polymer
 construction
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              2387
_journal_paper_doi               10.1039/b302807k
_journal_year                    2003
_chemical_formula_moiety         'C12 H10 N4 Ni O7, C12 H8 N2, 0.9(H2 O)'
_chemical_formula_sum            'C24 H19.8 N6 Ni O7.9'
_chemical_formula_weight         577.37
_chemical_name_common            '[Ni(NO3)2(H2O)(4,7-phen)].(4,7-phen)'
_chemical_name_systematic
; 
Aquabis(nitrato)(4,7-phenanthroline)nickel(II) 
4,7-phenanthroline water 1/1/0.9
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens
'those on water molecule, found from delta-F; others placed geometrically'
_atom_sites_solution_primary     'Patterson map'
_atom_sites_solution_secondary   'difference Fourier synthesis'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.107(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3438(13)
_cell_length_b                   7.9690(7)
_cell_length_c                   21.943(2)
_cell_measurement_reflns_used    1844
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.75
_cell_volume                     2519.5(4)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_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  0.049
_diffrn_reflns_av_sigmaI/netI    0.078
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12631
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS version 2.03 (Bruker, 2001)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.45
_refine_diff_density_rms         0.10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment
'geometric restraints applied to water; others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5816
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.106
_refine_ls_R_factor_gt           0.0530
_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)+(0.064P)²+2.416P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.121
_refine_ls_wR_factor_ref         0.149
_reflns_number_gt                3615
_reflns_number_total             6217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302807k.txt
_cod_data_source_block           5(NIPHEN)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.064P)^2^+2.416P] where P==(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w==1/[\s^2^(Fo^2^)+(0.064P)^2^+2.416P] where P==(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C24 H19.80 N6 Ni O7.90'
_cod_database_code               7012933
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.67281(3) 0.84624(6) 0.67680(2) 0.01972(15) Uani 1 1 d . . .
N10 N 0.7908(3) 0.8803(5) 0.62203(17) 0.0355(9) Uani 1 1 d . . .
O1 O 0.81394(19) 0.8235(4) 0.67920(14) 0.0350(7) Uani 1 1 d . . .
O2 O 0.70555(18) 0.9187(4) 0.59571(13) 0.0288(7) Uani 1 1 d . . .
O3 O 0.8457(2) 0.8962(6) 0.59290(17) 0.0623(11) Uani 1 1 d . . .
N20 N 0.6817(2) 1.2171(4) 0.69350(16) 0.0289(8) Uani 1 1 d . . .
O4 O 0.70699(19) 1.0748(3) 0.72217(13) 0.0267(6) Uani 1 1 d . . .
O5 O 0.6288(2) 1.2238(4) 0.63697(13) 0.0351(7) Uani 1 1 d . . .
O6 O 0.7127(3) 1.3459(4) 0.72535(16) 0.0605(11) Uani 1 1 d . . .
O10 O 0.6487(2) 0.6086(4) 0.64003(14) 0.0290(7) Uani 1 1 d D . .
H11W H 0.651(4) 0.582(6) 0.6035(11) 0.073(19) Uiso 1 1 d D . .
H12W H 0.675(3) 0.529(5) 0.6646(19) 0.069(19) Uiso 1 1 d D . .
C1 C 0.7769(3) 0.6419(5) 0.89972(19) 0.0283(9) Uani 1 1 d . . .
H1A H 0.8018 0.6049 0.9435 0.034 Uiso 1 1 calc R . .
C2 C 0.8308(3) 0.7340(5) 0.87330(19) 0.0287(9) Uani 1 1 d . . .
H2A H 0.8935 0.7600 0.8980 0.034 Uiso 1 1 calc R . .
C3 C 0.7911(3) 0.7883(5) 0.80909(19) 0.0260(9) Uani 1 1 d . . .
H3A H 0.8283 0.8540 0.7914 0.031 Uiso 1 1 calc R . .
N4 N 0.7045(2) 0.7542(4) 0.77110(14) 0.0208(7) Uani 1 1 d . . .
C5 C 0.5584(2) 0.6179(5) 0.75709(17) 0.0197(8) Uani 1 1 d . . .
H5A H 0.5362 0.6529 0.7130 0.024 Uiso 1 1 calc R . .
C6 C 0.5019(3) 0.5302(5) 0.78112(17) 0.0216(8) Uani 1 1 d . . .
H6A H 0.4409 0.5029 0.7533 0.026 Uiso 1 1 calc R . .
N7 N 0.4699(2) 0.3949(4) 0.86888(14) 0.0205(7) Uani 1 1 d . . .
C8 C 0.4979(3) 0.3504(5) 0.93151(17) 0.0227(8) Uani 1 1 d . . .
H8A H 0.4552 0.2940 0.9471 0.027 Uiso 1 1 calc R . .
C9 C 0.5869(3) 0.3830(5) 0.97507(18) 0.0235(8) Uani 1 1 d . . .
H9A H 0.6036 0.3497 1.0192 0.028 Uiso 1 1 calc R . .
C10 C 0.6500(3) 0.4634(5) 0.95368(17) 0.0235(8) Uani 1 1 d . . .
H10A H 0.7109 0.4860 0.9827 0.028 Uiso 1 1 calc R . .
C11 C 0.6514(3) 0.6584(5) 0.79748(17) 0.0210(8) Uani 1 1 d . . .
C12 C 0.6850(3) 0.6026(5) 0.86185(18) 0.0227(8) Uani 1 1 d . . .
C13 C 0.6235(3) 0.5120(5) 0.88823(17) 0.0206(8) Uani 1 1 d . . .
C14 C 0.5319(3) 0.4780(5) 0.84722(17) 0.0194(8) Uani 1 1 d . . .
C21 C 0.3446(3) 0.9715(5) 1.10891(19) 0.0292(9) Uani 1 1 d . . .
H21A H 0.3430 0.9464 1.1509 0.035 Uiso 1 1 calc R . .
C22 C 0.4209(3) 1.0481(5) 1.10242(19) 0.0281(9) Uani 1 1 d . . .
H22A H 0.4722 1.0787 1.1396 0.034 Uiso 1 1 calc R . .
C23 C 0.4218(3) 1.0801(5) 1.0403(2) 0.0287(9) Uani 1 1 d . . .
H23A H 0.4756 1.1305 1.0363 0.034 Uiso 1 1 calc R . .
N24 N 0.3521(2) 1.0445(5) 0.98631(16) 0.0316(8) Uani 1 1 d . A .
C25 C 0.2063(5) 0.9008(13) 0.9343(4) 0.027(2) Uiso 0.560(14) 1 d P A 1
H25A H 0.2158 0.9109 0.8939 0.033 Uiso 0.560(14) 1 calc PR A 1
C26 C 0.1297(6) 0.8234(13) 0.9367(4) 0.032(2) Uiso 0.560(14) 1 d P A 1
H26A H 0.0820 0.7938 0.8973 0.039 Uiso 0.560(14) 1 calc PR A 1
N27 N 0.0378(5) 0.7025(13) 0.9963(4) 0.039(2) Uiso 0.560(14) 1 d P A 1
C28 C 0.0297(7) 0.6671(16) 1.0530(5) 0.041(2) Uiso 0.560(14) 1 d P A 1
H28A H -0.0210 0.5994 1.0536 0.049 Uiso 0.560(14) 1 calc PR A 1
C25' C 0.1939(8) 0.9702(18) 0.9351(5) 0.034(3) Uiso 0.440(14) 1 d P A 2
H25B H 0.1957 1.0165 0.8956 0.041 Uiso 0.440(14) 1 calc PR A 2
C26' C 0.1144(9) 0.902(2) 0.9388(6) 0.045(3) Uiso 0.440(14) 1 d P A 2
H26B H 0.0618 0.8908 0.9004 0.054 Uiso 0.440(14) 1 calc PR A 2
N27' N 0.0261(7) 0.7804(17) 0.9964(5) 0.038(3) Uiso 0.440(14) 1 d P A 2
C28' C 0.0179(8) 0.7329(19) 1.0511(6) 0.036(3) Uiso 0.440(14) 1 d P A 2
H28B H -0.0421 0.7012 1.0503 0.043 Uiso 0.440(14) 1 calc PR A 2
C29 C 0.0921(3) 0.7246(8) 1.1121(2) 0.0518(14) Uani 1 1 d . . .
H29A H 0.0783 0.7098 1.1507 0.062 Uiso 1 1 calc R A 1
C30 C 0.1726(3) 0.8015(6) 1.1147(2) 0.0374(11) Uani 1 1 d . A .
H30A H 0.2193 0.8236 1.1554 0.045 Uiso 1 1 calc R . .
C31 C 0.2750(3) 0.9695(6) 0.99269(19) 0.0324(10) Uani 1 1 d . . .
C32 C 0.2688(3) 0.9303(5) 1.05352(18) 0.0256(9) Uani 1 1 d . A .
C33 C 0.1858(3) 0.8482(6) 1.0566(2) 0.0324(10) Uani 1 1 d . . .
C34 C 0.1185(6) 0.7838(15) 0.9988(4) 0.033(2) Uiso 0.560(14) 1 d P A 1
C34' C 0.1085(8) 0.8491(18) 0.9984(5) 0.033(3) Uiso 0.440(14) 1 d P A 2
O1W O 1.0549(12) 0.757(3) 0.7708(9) 0.073(5) Uiso 0.25 1 d P B 1
O2W O 1.0194(13) 1.021(3) 0.7591(9) 0.079(5) Uiso 0.25 1 d P C 1
O1WA O 1.0267(15) 0.658(3) 0.7609(10) 0.063(5) Uiso 0.20 1 d P D 2
O2WA O 1.0381(14) 0.915(3) 0.7634(10) 0.059(5) Uiso 0.20 1 d P E 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'
Ni Ni 0.3393 1.1124 '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
_geom_angle_publ_flag
O10 Ni1 O4 174.10(12) . . y
O10 Ni1 N4 90.84(12) . . y
O4 Ni1 N4 84.13(12) . . y
O10 Ni1 O2 89.07(12) . . y
O4 Ni1 O2 94.10(11) . . y
N4 Ni1 O2 153.91(11) . . y
O10 Ni1 N7 88.00(12) . 2_656 y
O4 Ni1 N7 96.77(12) . 2_656 y
N4 Ni1 N7 112.71(11) . 2_656 y
O2 Ni1 N7 93.36(11) . 2_656 y
O10 Ni1 O1 88.60(12) . . y
O4 Ni1 O1 88.61(12) . . y
N4 Ni1 O1 93.23(11) . . y
O2 Ni1 O1 60.69(10) . . y
N7 Ni1 O1 153.88(11) 2_656 . y
O3 N10 O1 123.0(4) . . ?
O3 N10 O2 121.4(4) . . ?
O1 N10 O2 115.5(3) . . ?
N10 O1 Ni1 90.5(2) . . ?
N10 O2 Ni1 93.3(2) . . ?
O5 N20 O6 121.6(3) . . ?
O5 N20 O4 121.0(3) . . ?
O6 N20 O4 117.4(3) . . ?
N20 O4 Ni1 124.0(2) . . ?
C2 C1 C12 119.8(4) . . ?
C1 C2 C3 118.2(4) . . ?
N4 C3 C2 124.3(4) . . ?
C3 N4 C11 117.1(3) . . ?
C3 N4 Ni1 113.0(2) . . ?
C11 N4 Ni1 129.7(2) . . ?
C6 C5 C11 120.7(3) . . ?
C5 C6 C14 121.4(3) . . ?
C8 N7 C14 117.8(3) . . ?
C8 N7 Ni1 110.8(2) . 2_646 ?
C14 N7 Ni1 130.9(2) . 2_646 ?
N7 C8 C9 123.2(3) . . ?
C10 C9 C8 119.5(3) . . ?
C9 C10 C13 119.2(3) . . ?
N4 C11 C12 122.2(3) . . ?
N4 C11 C5 118.1(3) . . ?
C12 C11 C5 119.7(3) . . ?
C11 C12 C1 118.3(3) . . ?
C11 C12 C13 119.6(3) . . ?
C1 C12 C13 122.1(3) . . ?
C10 C13 C14 118.3(3) . . ?
C10 C13 C12 122.8(3) . . ?
C14 C13 C12 118.8(3) . . ?
N7 C14 C13 122.0(3) . . ?
N7 C14 C6 118.3(3) . . ?
C13 C14 C6 119.7(3) . . ?
C22 C21 C32 119.8(4) . . ?
C21 C22 C23 118.7(4) . . ?
N24 C23 C22 124.0(4) . . ?
C23 N24 C31 117.4(3) . . ?
C26 C25 C31 121.2(7) . . ?
C25 C26 C34 121.2(8) . . ?
C28 N27 C34 115.9(8) . . ?
N27 C28 C29 123.1(9) . . ?
C26' C25' C31 117.9(10) . . ?
C25' C26' C34' 121.3(11) . . ?
C28' N27' C34' 117.9(10) . . ?
N27' C28' C29 125.2(10) . . ?
C30 C29 C28 120.6(6) . . ?
C30 C29 C28' 115.9(6) . . ?
C28 C29 C28' 22.4(6) . . ?
C29 C30 C33 119.5(4) . . ?
N24 C31 C32 122.4(4) . . ?
N24 C31 C25' 115.1(6) . . ?
C32 C31 C25' 121.0(6) . . ?
N24 C31 C25 117.5(4) . . ?
C32 C31 C25 119.1(5) . . ?
C25' C31 C25 23.4(5) . . ?
C21 C32 C31 117.7(4) . . ?
C21 C32 C33 122.9(4) . . ?
C31 C32 C33 119.4(4) . . ?
C30 C33 C34' 118.8(6) . . ?
C30 C33 C34 115.1(5) . . ?
C34' C33 C34 22.0(5) . . ?
C30 C33 C32 124.2(4) . . ?
C34' C33 C32 115.6(6) . . ?
C34 C33 C32 119.9(5) . . ?
N27 C34 C33 124.6(7) . . ?
N27 C34 C26 117.1(8) . . ?
C33 C34 C26 117.9(7) . . ?
N27' C34' C26' 116.5(10) . . ?
N27' C34' C33 120.5(9) . . ?
C26' C34' C33 122.7(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O10 2.042(3) . y
Ni1 O4 2.055(3) . y
Ni1 N4 2.089(3) . y
Ni1 O2 2.090(3) . y
Ni1 N7 2.107(3) 2_656 y
Ni1 O1 2.156(3) . y
N10 O3 1.227(4) . ?
N10 O1 1.264(4) . ?
N10 O2 1.272(4) . ?
N20 O5 1.228(4) . ?
N20 O6 1.241(4) . ?
N20 O4 1.290(4) . ?
C1 C2 1.374(5) . ?
C1 C12 1.404(5) . ?
C2 C3 1.398(5) . ?
C3 N4 1.331(5) . ?
N4 C11 1.380(5) . ?
C5 C6 1.354(5) . ?
C5 C11 1.434(5) . ?
C6 C14 1.425(5) . ?
N7 C8 1.339(5) . ?
N7 C14 1.372(4) . ?
N7 Ni1 2.107(3) 2_646 ?
C8 C9 1.395(5) . ?
C9 C10 1.372(5) . ?
C10 C13 1.406(5) . ?
C11 C12 1.399(5) . ?
C12 C13 1.458(5) . ?
C13 C14 1.410(5) . ?
C21 C22 1.371(6) . ?
C21 C32 1.402(6) . ?
C22 C23 1.392(5) . ?
C23 N24 1.325(5) . ?
N24 C31 1.374(5) . ?
C25 C26 1.343(11) . ?
C25 C31 1.458(9) . ?
C26 C34 1.465(11) . ?
N27 C28 1.322(12) . ?
N27 C34 1.383(11) . ?
C28 C29 1.398(11) . ?
C25' C26' 1.363(15) . ?
C25' C31 1.437(12) . ?
C26' C34' 1.407(16) . ?
N27' C28' 1.304(14) . ?
N27' C34' 1.365(14) . ?
C28' C29 1.430(13) . ?
C29 C30 1.362(6) . ?
C30 C33 1.408(6) . ?
C31 C32 1.406(5) . ?
C32 C33 1.453(6) . ?
C33 C34' 1.413(12) . ?
C33 C34 1.428(10) . ?
