#------------------------------------------------------------------------------
#$Date: 2019-10-09 07:05:03 +0300 (Wed, 09 Oct 2019) $
#$Revision: 219184 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/31/2243133.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_2243133
loop_
_publ_author_name
'Simões, Andrea B.'
'Figueira, Flávio'
'Mendes, Ricardo F.'
'Barbosa, Jéssica S.'
'Rocha, João'
'Paz, Filipe A. Almeida'
_publ_section_title
;
 One-dimensional ladder gallium coordination polymer
;
_journal_coeditor_code           SJ5578
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1607
_journal_page_last               1612
_journal_paper_doi               10.1107/S2056989019013446
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Ga (C5 H2 N2 O4) (O H) (H2 O)]'
_chemical_formula_moiety         'C5 H5 Ga N2 O6'
_chemical_formula_sum            'C5 H5 Ga N2 O6'
_chemical_formula_weight         258.83
_chemical_name_systematic
'Poly[[(μ₂-hydroxido)(μ₂-1H-pyrazole-3,5-dicarboxylato)gallium(III)] monohydrate]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'SHELXL-2018/3, manual editing plus enCIFer'
_cell_angle_alpha                94.804(8)
_cell_angle_beta                 101.306(7)
_cell_angle_gamma                108.596(7)
_cell_formula_units_Z            2
_cell_length_a                   6.6055(13)
_cell_length_b                   6.8830(16)
_cell_length_c                   8.5178(19)
_cell_measurement_reflns_used    3255
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.47
_cell_volume                     355.44(14)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 QUEST '
_diffrn_measurement_method       'ω / φ scans'
_diffrn_radiation_monochromator  'Multi-layer X-ray mirror'
_diffrn_radiation_source         'Sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5768
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.393
_diffrn_reflns_theta_min         3.663
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001; Krause et al. 2015)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.418
_exptl_crystal_description       Block
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.467
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1303
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0312
_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)+(0.0292P)²+1.2151P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                1182
_reflns_number_total             1303
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            sj5578sup1.cif
_cod_data_source_block           I
_cod_database_code               2243133
_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.
;
_shelx_estimated_absorpt_t_min   0.632
_shelx_estimated_absorpt_t_max   0.773
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_occupancy
Ga Ga1 0.20874(7) 0.17985(7) 1.03804(5) 0.00844(15) Uani d 1
O O1W 0.5321(4) 0.2428(4) 1.0908(3) 0.0140(6) Uani d 1
H H1X 0.604(6) 0.162(6) 1.147(5) 0.021 Uiso d 1
H H1Y 0.627(5) 0.335(5) 1.040(5) 0.021 Uiso d 1
O O1 0.1126(4) -0.1152(4) 1.0094(3) 0.0100(6) Uani d 1
H H1 0.142(8) -0.167(7) 1.082(6) 0.015 Uiso d 1
N N1 0.2437(5) 0.1027(5) 0.4128(4) 0.0102(7) Uani d 1
H H1N 0.249943 -0.023469 0.404671 0.012 Uiso calc 1
N N2 0.2363(5) 0.2116(5) 0.2909(4) 0.0088(7) Uani d 1
C C1 0.2537(6) 0.1216(6) 0.7048(5) 0.0103(8) Uani d 1
C C2 0.2405(6) 0.2131(6) 0.5511(4) 0.0089(8) Uani d 1
C C3 0.2296(6) 0.4004(6) 0.5154(5) 0.0102(8) Uani d 1
H H3 0.223752 0.511146 0.586837 0.012 Uiso calc 1
C C4 0.2289(6) 0.3927(6) 0.3507(4) 0.0074(8) Uani d 1
C C5 0.2388(6) 0.5450(6) 0.2360(5) 0.0087(8) Uani d 1
O O2 0.2500(4) 0.4783(4) 0.0937(3) 0.0098(6) Uani d 1
O O3 0.2423(5) 0.7207(4) 0.2790(3) 0.0137(6) Uani d 1
O O4 0.2886(5) -0.0428(4) 0.7039(3) 0.0149(6) Uani d 1
O O5 0.2257(4) 0.2323(4) 0.8208(3) 0.0123(6) Uani 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'
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'
Ga Ga 0.2307 1.6083 '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'
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
O1 Ga1 O5 . . 101.59(12) yes
O1 Ga1 O1 . 2_557 79.94(13) yes
O5 Ga1 O1 . 2_557 93.13(12) yes
O1 Ga1 O2 . 1_556 166.31(11) yes
O5 Ga1 O2 . 1_556 87.28(11) yes
O1 Ga1 O2 2_557 1_556 89.26(11) yes
O1 Ga1 O1W . . 99.60(12) yes
O5 Ga1 O1W . . 88.20(12) yes
O1 Ga1 O1W 2_557 . 178.65(12) yes
O2 Ga1 O1W 1_556 . 91.00(11) yes
O1 Ga1 N2 . 1_556 93.94(12) yes
O5 Ga1 N2 . 1_556 164.18(12) yes
O1 Ga1 N2 2_557 1_556 92.49(12) yes
O2 Ga1 N2 1_556 1_556 78.02(11) yes
O1W Ga1 N2 . 1_556 86.27(12) yes
O1 Ga1 Ga1 . 2_557 40.86(8) ?
O5 Ga1 Ga1 . 2_557 99.50(8) ?
O1 Ga1 Ga1 2_557 2_557 39.08(8) ?
O2 Ga1 Ga1 1_556 2_557 127.84(8) ?
O1W Ga1 Ga1 . 2_557 140.45(9) ?
N2 Ga1 Ga1 1_556 2_557 94.18(9) ?
Ga1 O1W H1X . . 124(2) ?
Ga1 O1W H1Y . . 123(2) ?
H1X O1W H1Y . . 110.8(16) ?
Ga1 O1 Ga1 . 2_557 100.06(13) ?
Ga1 O1 H1 . . 118(4) ?
Ga1 O1 H1 2_557 . 107(4) ?
N2 N1 C2 . . 110.6(3) ?
N2 N1 H1N . . 124.7 ?
C2 N1 H1N . . 124.7 ?
C4 N2 N1 . . 106.8(3) ?
C4 N2 Ga1 . 1_554 112.3(2) ?
N1 N2 Ga1 . 1_554 140.7(3) ?
O4 C1 O5 . . 129.1(4) ?
O4 C1 C2 . . 118.2(3) ?
O5 C1 C2 . . 112.7(3) ?
N1 C2 C3 . . 107.5(3) ?
N1 C2 C1 . . 119.5(3) ?
C3 C2 C1 . . 133.0(4) ?
C2 C3 C4 . . 104.8(3) ?
C2 C3 H3 . . 127.6 ?
C4 C3 H3 . . 127.6 ?
N2 C4 C3 . . 110.3(3) ?
N2 C4 C5 . . 115.1(3) ?
C3 C4 C5 . . 134.4(3) ?
O3 C5 O2 . . 124.3(4) ?
O3 C5 C4 . . 121.2(3) ?
O2 C5 C4 . . 114.5(3) ?
C5 O2 Ga1 . 1_554 118.6(2) ?
C1 O5 Ga1 . . 129.9(3) ?
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
Ga1 O1 . 1.903(3) yes
Ga1 O5 . 1.932(3) yes
Ga1 O1 2_557 1.974(3) yes
Ga1 O2 1_556 1.987(3) yes
Ga1 O1W . 1.988(3) yes
Ga1 N2 1_556 2.112(3) yes
Ga1 Ga1 2_557 2.9716(10) ?
O1W H1X . 0.943(10) ?
O1W H1Y . 0.939(10) ?
O1 H1 . 0.77(5) ?
N1 N2 . 1.333(4) ?
N1 C2 . 1.355(5) ?
N1 H1N . 0.8800 ?
N2 C4 . 1.326(5) ?
C1 O4 . 1.224(5) ?
C1 O5 . 1.276(5) ?
C1 C2 . 1.499(5) ?
C2 C3 . 1.369(6) ?
C3 C4 . 1.399(5) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.487(5) ?
C5 O3 . 1.225(5) ?
C5 O2 . 1.284(5) ?
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
O1W H1X O4 2_657 0.943 1.725 2.643(4) 164 yes
O1W H1Y O2 2_666 0.939 1.885 2.803(4) 165 yes
O1 H1 O3 1_546 0.77 1.99 2.751(4) 175 yes
N1 H1N O3 1_545 0.88 1.96 2.773(4) 152.4 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
C2 N1 N2 C4 . . 0.2(4)
C2 N1 N2 Ga1 . 1_554 -173.6(3)
N2 N1 C2 C3 . . 0.2(4)
N2 N1 C2 C1 . . -178.4(3)
O4 C1 C2 N1 . . 7.0(5)
O5 C1 C2 N1 . . -173.1(3)
O4 C1 C2 C3 . . -171.2(4)
O5 C1 C2 C3 . . 8.7(6)
N1 C2 C3 C4 . . -0.5(4)
C1 C2 C3 C4 . . 177.8(4)
N1 N2 C4 C3 . . -0.5(4)
Ga1 N2 C4 C3 1_554 . 175.2(2)
N1 N2 C4 C5 . . 175.1(3)
Ga1 N2 C4 C5 1_554 . -9.2(4)
C2 C3 C4 N2 . . 0.7(4)
C2 C3 C4 C5 . . -173.7(4)
N2 C4 C5 O3 . . -177.0(3)
C3 C4 C5 O3 . . -2.8(7)
N2 C4 C5 O2 . . 1.0(5)
C3 C4 C5 O2 . . 175.2(4)
O3 C5 O2 Ga1 . 1_554 -173.3(3)
C4 C5 O2 Ga1 . 1_554 8.8(4)
O4 C1 O5 Ga1 . . -4.2(6)
C2 C1 O5 Ga1 . . 175.8(2)

_cod_database_fobs_code 2243133
