#------------------------------------------------------------------------------
#$Date: 2024-12-07 19:03:28 +0200 (Sat, 07 Dec 2024) $
#$Revision: 296756 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312706.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_2312706
loop_
_publ_author_name
'Moya, Marielsys'
'Liendo-Polanco, Gustavo R'
'Atencio, Reinaldo'
'Silva, Pedro'
'Henao, Jose A.'
'Bruno-Colmenares, Julia'
_publ_section_title
;
 Coordination geometry flexibility driving supramolecular isomerism of
 Cu/Mo pillared-layer hybrid networks.
;
_journal_issue                   6
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              782
_journal_page_last               792
_journal_paper_doi               10.1107/S2052520624009934
_journal_volume                  80
_journal_year                    2024
_chemical_formula_moiety         'C10 H8 Cu2 Mo2 N2 O8, 0.5[H2O]'
_chemical_formula_sum            'C10 H9 Cu2 Mo2 N2 O8.5'
_chemical_formula_weight         612.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                95.990(2)
_cell_angle_beta                 93.999(2)
_cell_angle_gamma                110.227(2)
_cell_formula_units_Z            1
_cell_length_a                   5.61200(10)
_cell_length_b                   5.77240(10)
_cell_length_c                   12.4665(3)
_cell_measurement_reflns_used    7624
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.3864
_cell_measurement_theta_min      1.8298
_cell_volume                     374.444(14)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Area detector'
_diffrn_detector_type            'Rigaku Pilatus 200'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'XtaLAB (RCD3): quarter-chi single'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200 AFC11'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'Curve graphite monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2662
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.549
_diffrn_reflns_theta_max         66.549
_diffrn_reflns_theta_min         7.190
_diffrn_source                   'Microfocus Cu-radiation'
_diffrn_source_target            Cu
_exptl_absorpt_coefficient_mu    17.085
_exptl_absorpt_correction_T_max  0.108
_exptl_absorpt_correction_T_min  0.094
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   DTABSCOR
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.715
_exptl_crystal_description       block
_exptl_crystal_F_000             293
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0275
_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)+(0.0447P)²+0.3926P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1283
_reflns_number_total             1295
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            yv5021sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2312705--2312708.cif.'
_cod_original_cell_volume        374.443(14)
_cod_original_formula_sum        'C10 H9 Cu2 Mo2 N2 O8.50'
_cod_database_code               2312706
_cod_database_fobs_code          2312706
_shelx_shelxl_version_number     2018/3
_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_max   0.100
_shelx_estimated_absorpt_t_min   0.087
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 5 electrons were 
found in a volume of 19Å³ in 1 void per unit cell. 
This is consistent with the presence of 0.25[H2O] per 
Asymmetric Unit which account for 5 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.45736(5) 0.15076(5) 0.87971(2) 0.01195(14) Uani 1 1 d . . . . .
Cu1 Cu 0.87732(10) 0.76837(10) 0.92378(4) 0.01341(17) Uani 1 1 d . . . . .
O1 O 0.7047(5) 0.4246(5) 0.9441(2) 0.0196(6) Uani 1 1 d . . . . .
O2 O 0.4293(6) 0.1713(6) 0.7440(2) 0.0264(7) Uani 1 1 d . . . . .
O3 O 0.1370(5) 0.1072(5) 0.9250(2) 0.0147(5) Uani 1 1 d . . . . .
O4 O 0.5412(5) -0.1102(5) 0.8924(2) 0.0204(6) Uani 1 1 d . . . . .
N1 N 0.9138(6) 0.6691(6) 0.7714(3) 0.0176(7) Uani 1 1 d . . . . .
C1 C 1.0403(8) 0.5156(8) 0.7479(3) 0.0225(9) Uani 1 1 d . . . . .
H1 H 1.104975 0.452815 0.804261 0.027 Uiso 1 1 calc R U . . .
C2 C 1.0784(9) 0.4469(9) 0.6423(3) 0.0260(9) Uani 1 1 d . . . . .
H2 H 1.168872 0.340966 0.628851 0.031 Uiso 1 1 calc R U . . .
C4 C 0.8472(10) 0.6925(10) 0.5830(4) 0.0335(11) Uani 1 1 d . . . . .
H4 H 0.777206 0.755554 0.528287 0.040 Uiso 1 1 calc R U . . .
C5 C 0.8182(10) 0.7534(9) 0.6893(4) 0.0286(10) Uani 1 1 d . . . . .
H5 H 0.727754 0.858390 0.704943 0.034 Uiso 1 1 calc R U . . .
C3 C 0.9820(8) 0.5356(8) 0.5573(3) 0.0208(9) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O1 Mo1 O3 114.40(12) . . ?
O2 Mo1 O1 107.67(14) . . ?
O2 Mo1 O3 106.41(13) . . ?
O2 Mo1 O4 106.22(15) . . ?
O4 Mo1 O1 110.41(13) . . ?
O4 Mo1 O3 111.26(13) . . ?
O1 Cu1 Cu1 132.99(9) . 2_777 ?
O1 Cu1 O3 163.93(12) . 1_665 ?
O1 Cu1 O3 92.78(12) . 2_667 ?
O1 Cu1 O4 100.77(11) . 1_565 ?
O1 Cu1 N1 91.55(13) . . ?
O3 Cu1 Cu1 42.21(8) 2_667 2_777 ?
O3 Cu1 Cu1 41.45(7) 1_665 2_777 ?
O3 Cu1 O3 83.65(11) 2_667 1_665 ?
O3 Cu1 O4 94.35(11) 1_665 1_565 ?
O3 Cu1 O4 82.94(11) 2_667 1_565 ?
O3 Cu1 N1 175.41(13) 2_667 . ?
O4 Cu1 Cu1 88.25(8) 1_565 2_777 ?
N1 Cu1 Cu1 133.21(10) . 2_777 ?
N1 Cu1 O3 91.76(12) . 1_665 ?
N1 Cu1 O4 97.73(13) . 1_565 ?
Mo1 O1 Cu1 140.44(17) . . ?
Mo1 O3 Cu1 117.95(13) . 2_667 ?
Mo1 O3 Cu1 121.33(14) . 1_445 ?
Cu1 O3 Cu1 96.35(11) 2_667 1_445 ?
Mo1 O4 Cu1 143.08(15) . 1_545 ?
C1 N1 Cu1 120.0(3) . . ?
C5 N1 Cu1 122.0(3) . . ?
C5 N1 C1 118.0(4) . . ?
N1 C1 H1 118.9 . . ?
N1 C1 C2 122.2(4) . . ?
C2 C1 H1 118.9 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 H2 120.0 . . ?
C5 C4 H4 120.2 . . ?
C5 C4 C3 119.7(4) . . ?
C3 C4 H4 120.2 . . ?
N1 C5 C4 123.0(4) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C2 C3 C4 117.1(4) . . ?
C2 C3 C3 121.4(5) . 2_766 ?
C4 C3 C3 121.5(5) . 2_766 ?
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
Mo1 O1 1.770(3) . ?
Mo1 O2 1.709(3) . ?
Mo1 O3 1.864(3) . ?
Mo1 O4 1.745(3) . ?
Cu1 Cu1 2.9474(10) 2_777 ?
Cu1 O1 1.936(3) . ?
Cu1 O3 1.992(3) 1_665 ?
Cu1 O3 1.963(3) 2_667 ?
Cu1 O4 2.252(3) 1_565 ?
Cu1 N1 1.972(3) . ?
N1 C1 1.335(6) . ?
N1 C5 1.334(6) . ?
C1 H1 0.9300 . ?
C1 C2 1.388(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.380(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.371(6) . ?
C4 C3 1.394(6) . ?
C5 H5 0.9300 . ?
C3 C3 1.491(8) 2_766 ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 N1 C1 C2 -177.8(4) . . . . ?
Cu1 N1 C5 C4 178.2(4) . . . . ?
O1 Mo1 O3 Cu1 -32.42(19) . . . 2_667 ?
O1 Mo1 O3 Cu1 -150.41(15) . . . 1_445 ?
O1 Mo1 O4 Cu1 -21.3(3) . . . 1_545 ?
O2 Mo1 O1 Cu1 25.0(3) . . . . ?
O2 Mo1 O3 Cu1 -151.18(16) . . . 2_667 ?
O2 Mo1 O3 Cu1 90.82(18) . . . 1_445 ?
O2 Mo1 O4 Cu1 95.2(3) . . . 1_545 ?
O3 Mo1 O1 Cu1 -93.0(3) . . . . ?
O3 Mo1 O4 Cu1 -149.4(2) . . . 1_545 ?
O4 Mo1 O1 Cu1 140.6(2) . . . . ?
O4 Mo1 O3 Cu1 -24.45(19) . . . 1_445 ?
O4 Mo1 O3 Cu1 93.55(17) . . . 2_667 ?
N1 C1 C2 C3 -0.7(7) . . . . ?
C1 N1 C5 C4 -0.9(7) . . . . ?
C1 C2 C3 C4 -0.3(7) . . . . ?
C1 C2 C3 C3 -179.7(5) . . . 2_766 ?
C5 N1 C1 C2 1.3(7) . . . . ?
C5 C4 C3 C2 0.6(8) . . . . ?
C5 C4 C3 C3 180.0(5) . . . 2_766 ?
C3 C4 C5 N1 0.0(8) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 19.1 4.8 '0.5 water'
