#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:51:08 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228950 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/10/7231094.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_7231094
loop_
_publ_author_name
'Briones, David'
'Leo, Pedro'
'Cepeda, Javier'
'Orcajo, Gisela'
'Calleja, Guillermo'
'Sanz, Raúl'
'Rodríguez-Diéguez, Antonio'
'Martínez, Fernando'
_publ_section_title
;
 Alkaline-earth metal based MOFs with second scale long-lasting phosphor
 behavior
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4793
_journal_paper_doi               10.1039/C8CE00479J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C11 H13 Ca N O6, 2 (H2 O)'
_chemical_formula_sum            'C11 H17 Ca N O8'
_chemical_formula_weight         331.33
_chemical_name_systematic
"poly-{[diaqua(mu-1,4-benzenedicarboxylate-k2O,O':k2O'',O''')(mu6-1,4-benzenedicarboxylate-?O:?2O,O':?O':?O'':?2O'',O''':?O''' ) bis(dimethylformamide)dicalcium(II)] tetrahydrate}"
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-06-10 deposited with the CCDC.
2018-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.17(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.540(5)
_cell_length_b                   6.683(5)
_cell_length_c                   19.460(5)
_cell_measurement_reflns_used    7661
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.760
_cell_measurement_theta_min      2.332
_cell_volume                     1463.7(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       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  0.0244
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7661
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.760
_diffrn_reflns_theta_min         2.332
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    none
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             696
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
TITL shelx     P 21/c       R = 0.08
CELL   12.5400    6.6830   19.4600     90.00    116.17     90.00
SPGR P21/c
# Solvent Accessible Volume =       212
# Electrons Found in S.A.V. =        45
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.372 0.547 0.300 !       4.78 eA-3
Q102 0.424 0.530 0.238 !       2.51 eA-3
Q103 0.340 0.462 0.643 !       2.02 eA-3
Q104 0.279 1.017 0.172 !       1.98 eA-3
C105 0.485 0.297 0.292 !       1.56 eA-3
Q106 0.454 0.946 0.159 !       1.43 eA-3
Q107 0.326 0.536 0.246 !       1.43 eA-3
Q108 0.515 0.400 0.262 !       1.17 eA-3
C109 0.558 0.265 0.282 !       0.86 eA-3
Q110 0.595 0.895 0.224 !       0.83 eA-3
C111 0.592 0.147 0.219 !       0.82 eA-3
Q112 0.512 0.503 0.215 !       0.72 eA-3
;
_refine_diff_density_max         1.952
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0869P)²+2.1275P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3243
_reflns_number_total             3752
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00479j2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
'Adding full bibliography for 7231092--7231094.cif.'
_cod_database_code               7231094
_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.
;
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.05758(3) 0.47144(6) 0.72523(2) 0.00749(14) Uani 1 1 d . . . .
C1A C -0.01430(17) 0.4740(3) 0.84728(11) 0.0076(4) Uani 1 1 d . . . .
C2A C -0.00670(18) 0.4872(3) 0.92649(12) 0.0098(4) Uani 1 1 d . . . .
C3A C -0.0416(2) 0.3256(3) 0.95748(12) 0.0146(4) Uani 1 1 d . . . .
H3A H -0.0693 0.2089 0.9291 0.018 Uiso 1 1 calc R U . .
C4A C 0.0351(2) 0.6614(3) 0.96953(12) 0.0141(4) Uani 1 1 d . . . .
H4A H 0.0587 0.7692 0.9493 0.017 Uiso 1 1 calc R U . .
C1B C 0.28343(19) 0.4782(3) 0.85812(13) 0.0131(4) Uani 1 1 d . . . .
C2B C 0.39543(19) 0.4892(3) 0.93175(13) 0.0133(4) Uani 1 1 d . . . .
C4B C 0.4610(2) 0.3171(3) 0.96425(13) 0.0182(5) Uani 1 1 d . . . .
H4B H 0.4349 0.1941 0.9404 0.022 Uiso 1 1 calc R U . .
C3B C 0.4353(2) 0.6721(3) 0.96812(13) 0.0179(5) Uani 1 1 d . . . .
H3B H 0.3921 0.7879 0.9469 0.022 Uiso 1 1 calc R U . .
O1A O -0.01192(14) 0.6332(2) 0.81347(8) 0.0118(3) Uani 1 1 d . . . .
O2A O -0.01841(14) 0.3056(2) 0.81783(8) 0.0123(3) Uani 1 1 d . . . .
O1B O 0.23588(15) 0.6382(3) 0.82491(10) 0.0214(4) Uani 1 1 d . . . .
O2B O 0.24048(16) 0.3105(3) 0.83073(10) 0.0245(4) Uani 1 1 d . . . .
O1C O 0.17624(15) 0.4435(3) 0.65909(10) 0.0192(4) Uani 1 1 d . . . .
C2C C 0.2348(3) 0.2953(5) 0.65903(18) 0.0339(6) Uani 1 1 d . . A 1
H2C H 0.2423 0.1937 0.6935 0.041 Uiso 1 1 calc R U A 1
N3C N 0.2879(3) 0.2682(5) 0.61420(19) 0.0495(8) Uani 1 1 d . . A 1
C4C C 0.2785(4) 0.4082(8) 0.5579(3) 0.0712(16) Uani 1 1 d . . A 1
H4C1 H 0.2314 0.3528 0.5080 0.107 Uiso 1 1 calc R U A 1
H4C2 H 0.3563 0.4397 0.5630 0.107 Uiso 1 1 calc R U A 1
H4C3 H 0.2413 0.5278 0.5642 0.107 Uiso 1 1 calc R U A 1
C5C C 0.3500(5) 0.0802(8) 0.6166(3) 0.0790(16) Uani 1 1 d . . A 1
H5C1 H 0.3402 -0.0108 0.6516 0.118 Uiso 1 1 calc R U A 1
H5C2 H 0.4330 0.1067 0.6335 0.118 Uiso 1 1 calc R U A 1
H5C3 H 0.3174 0.0217 0.5665 0.118 Uiso 1 1 calc R U A 1
O1W O -0.14849(14) 0.4717(2) 0.63434(9) 0.0137(3) Uani 1 1 d . . B 1
H1W1 H -0.1850 0.3740 0.6388 0.021 Uiso 1 1 d . U C 1
H2W1 H -0.1848 0.5709 0.6369 0.021 Uiso 1 1 d . U D 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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'
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
O2A Ca1 O1C 87.93(6) 2_556 .
O2A Ca1 O1A 143.71(6) 2_556 2_546
O1C Ca1 O1A 82.75(6) . 2_546
O2A Ca1 O1W 75.53(5) 2_556 .
O1C Ca1 O1W 109.26(7) . .
O1A Ca1 O1W 74.70(5) 2_546 .
O2A Ca1 O1B 80.08(6) 2_556 .
O1C Ca1 O1B 83.96(7) . .
O1A Ca1 O1B 133.10(6) 2_546 .
O1W Ca1 O1B 151.56(6) . .
O2A Ca1 O1A 75.67(6) 2_556 .
O1C Ca1 O1A 154.86(6) . .
O1A Ca1 O1A 121.60(4) 2_546 .
O1W Ca1 O1A 85.27(6) . .
O1B Ca1 O1A 74.64(6) . .
O2A Ca1 O2B 131.21(6) 2_556 .
O1C Ca1 O2B 81.16(7) . .
O1A Ca1 O2B 81.89(6) 2_546 .
O1W Ca1 O2B 152.61(6) . .
O1B Ca1 O2B 51.65(7) . .
O1A Ca1 O2B 95.29(7) . .
O2A Ca1 O2A 124.15(4) 2_556 .
O1C Ca1 O2A 147.75(6) . .
O1A Ca1 O2A 72.89(5) 2_546 .
O1W Ca1 O2A 84.69(6) . .
O1B Ca1 O2A 97.32(6) . .
O1A Ca1 O2A 50.71(6) . .
O2B Ca1 O2A 74.86(6) . .
O2A Ca1 C1B 105.85(6) 2_556 .
O1C Ca1 C1B 83.34(7) . .
O1A Ca1 C1B 107.76(6) 2_546 .
O1W Ca1 C1B 167.40(6) . .
O1B Ca1 C1B 25.83(6) . .
O1A Ca1 C1B 83.01(6) . .
O2B Ca1 C1B 25.91(6) . .
O2A Ca1 C1B 84.32(6) . .
O2A Ca1 C1A 101.23(5) 2_556 .
O1C Ca1 C1A 161.32(6) . .
O1A Ca1 C1A 98.49(5) 2_546 .
O1W Ca1 C1A 88.91(6) . .
O1B Ca1 C1A 81.67(6) . .
O1A Ca1 C1A 25.71(5) . .
O2B Ca1 C1A 80.57(7) . .
O2A Ca1 C1A 25.72(5) . .
C1B Ca1 C1A 78.52(7) . .
O2A Ca1 Ca1 148.36(5) 2_556 2_546
O1C Ca1 Ca1 117.02(5) . 2_546
O1A Ca1 Ca1 37.17(4) 2_546 2_546
O1W Ca1 Ca1 77.80(4) . 2_546
O1B Ca1 Ca1 119.45(5) . 2_546
O1A Ca1 Ca1 85.51(5) . 2_546
O2B Ca1 Ca1 74.96(5) . 2_546
O2A Ca1 Ca1 35.73(3) . 2_546
C1B Ca1 Ca1 96.65(5) . 2_546
C1A Ca1 Ca1 61.39(4) . 2_546
O2A Ca1 Ca1 40.54(4) 2_556 2_556
O1C Ca1 Ca1 126.06(5) . 2_556
O1A Ca1 Ca1 145.68(5) 2_546 2_556
O1W Ca1 Ca1 77.73(4) . 2_556
O1B Ca1 Ca1 74.25(5) . 2_556
O1A Ca1 Ca1 35.14(3) . 2_556
O2B Ca1 Ca1 117.38(5) . 2_556
O2A Ca1 Ca1 84.64(5) . 2_556
C1B Ca1 Ca1 95.11(5) . 2_556
C1A Ca1 Ca1 60.72(4) . 2_556
Ca1 Ca1 Ca1 116.70(5) 2_546 2_556
O2A C1A O1A 121.71(19) . .
O2A C1A C2A 119.48(17) . .
O1A C1A C2A 118.75(17) . .
O2A C1A Ca1 65.39(11) . .
O1A C1A Ca1 59.14(10) . .
C2A C1A Ca1 160.25(13) . .
C4A C2A C3A 119.48(19) . .
C4A C2A C1A 120.09(18) . .
C3A C2A C1A 120.43(18) . .
C4A C3A C2A 120.29(19) 3_567 .
C4A C3A H3A 119.9 3_567 .
C2A C3A H3A 119.9 . .
C3A C4A C2A 120.23(19) 3_567 .
C3A C4A H4A 119.9 3_567 .
C2A C4A H4A 119.9 . .
O1B C1B O2B 121.6(2) . .
O1B C1B C2B 118.8(2) . .
O2B C1B C2B 119.6(2) . .
O1B C1B Ca1 59.61(12) . .
O2B C1B Ca1 62.34(12) . .
C2B C1B Ca1 174.57(16) . .
C3B C2B C4B 119.2(2) . .
C3B C2B C1B 120.2(2) . .
C4B C2B C1B 120.6(2) . .
C3B C4B C2B 120.5(2) 3_667 .
C3B C4B H4B 119.7 3_667 .
C2B C4B H4B 119.7 . .
C4B C3B C2B 120.3(2) 3_667 .
C4B C3B H3B 119.8 3_667 .
C2B C3B H3B 119.8 . .
C1A O1A Ca1 156.06(14) . 2_556
C1A O1A Ca1 95.15(12) . .
Ca1 O1A Ca1 107.69(6) 2_556 .
C1A O2A Ca1 166.44(14) . 2_546
C1A O2A Ca1 88.89(12) . .
Ca1 O2A Ca1 103.74(6) 2_546 .
C1B O1B Ca1 94.56(14) . .
C1B O2B Ca1 91.75(14) . .
C2C O1C Ca1 125.57(18) . .
O1C C2C N3C 125.7(3) . .
O1C C2C H2C 117.1 . .
N3C C2C H2C 117.1 . .
C2C N3C C4C 121.9(3) . .
C2C N3C C5C 120.7(3) . .
C4C N3C C5C 117.1(3) . .
N3C C4C H4C1 109.5 . .
N3C C4C H4C2 109.5 . .
H4C1 C4C H4C2 109.5 . .
N3C C4C H4C3 109.5 . .
H4C1 C4C H4C3 109.5 . .
H4C2 C4C H4C3 109.5 . .
N3C C5C H5C1 109.5 . .
N3C C5C H5C2 109.5 . .
H5C1 C5C H5C2 109.5 . .
N3C C5C H5C3 109.5 . .
H5C1 C5C H5C3 109.5 . .
H5C2 C5C H5C3 109.5 . .
Ca1 O1W H1W1 112.9 . .
Ca1 O1W H2W1 113.7 . .
H1W1 O1W H2W1 106.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O2A 2.360(2) 2_556
Ca1 O1C 2.3653(18) .
Ca1 O1A 2.372(2) 2_546
Ca1 O1W 2.4032(19) .
Ca1 O1B 2.4856(19) .
Ca1 O1A 2.4893(16) .
Ca1 O2B 2.5454(19) .
Ca1 O2A 2.6264(16) .
Ca1 C1B 2.872(2) .
Ca1 C1A 2.888(2) .
Ca1 Ca1 3.925(2) 2_546
Ca1 Ca1 3.925(2) 2_556
C1A O2A 1.254(3) .
C1A O1A 1.258(3) .
C1A C2A 1.504(3) .
C2A C4A 1.394(3) .
C2A C3A 1.398(3) .
C3A C4A 1.389(3) 3_567
C3A H3A 0.9300 .
C4A C3A 1.389(3) 3_567
C4A H4A 0.9300 .
C1B O1B 1.256(3) .
C1B O2B 1.256(3) .
C1B C2B 1.502(3) .
C2B C3B 1.391(3) .
C2B C4B 1.393(3) .
C4B C3B 1.386(3) 3_667
C4B H4B 0.9300 .
C3B C4B 1.386(3) 3_667
C3B H3B 0.9300 .
O1A Ca1 2.372(2) 2_556
O2A Ca1 2.360(2) 2_546
O1C C2C 1.234(4) .
C2C N3C 1.323(4) .
C2C H2C 0.9300 .
N3C C4C 1.406(5) .
N3C C5C 1.468(5) .
C4C H4C1 0.9600 .
C4C H4C2 0.9600 .
C4C H4C3 0.9600 .
C5C H5C1 0.9600 .
C5C H5C2 0.9600 .
C5C H5C3 0.9600 .
O1W H1W1 0.8240 .
O1W H2W1 0.8180 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 -0.084 0.750 106 23 ' '
2 0.500 -0.041 0.250 107 23 ' '
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 1.809
-1 0 2 2.234
