Crystal Chemistry of the Copper Oxalate Biomineral Moolooite: The First Single-Crystal X-ray Diffraction Studies and Thermal Behavior.
Kornyakov, Ilya V.; Gurzhiy, Vladislav V.; Kuz'mina, Mariya A.; Krzhizhanovskaya, Maria G.; Chukanov, Nikita V.; Chislov, Mikhail V.; Korneev, Anatolii V.; Izatulina, Alina R.; International journal of molecular sciences 24 (2023) 6786–; doi:10.3390/ijms24076786

data_1569046
_publ_section_title
;
 Crystal Chemistry of the Copper Oxalate Biomineral Moolooite: The First
 Single-Crystal X-ray Diffraction Studies and Thermal Behavior.
;
_journal_issue                   7
_journal_name_full               'International journal of molecular sciences'
_journal_page_first              6786
_journal_paper_doi               10.3390/ijms24076786
_journal_volume                  24
_journal_year                    2023
_chemical_formula_moiety         'C2 Cu O4'
_chemical_formula_sum            'C2 Cu O4'
_chemical_formula_weight         151.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-24
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   5.601(2)
_cell_length_b                   5.415(3)
_cell_length_c                   2.5553(8)
_cell_measurement_reflns_used    386
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.7860
_cell_measurement_theta_min      5.2370
_cell_volume                     77.50(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     58.00  85.00   1.00  180.00    --   11.64  18.00-141.00   27
  2  \w    -54.00 -10.00   1.00  180.00    --   11.64 -18.00  50.00   44
  3  \w      8.00  52.00   1.00  180.00    --   11.64  18.00-141.00   44
  4  \w     -7.00  37.00   1.00  180.00    --   11.64  77.00 -90.00   44
  5  \w     41.00  81.00   1.00  180.00    --   11.64  77.00 -90.00   40
  6  \w      0.00  40.00   1.00  180.00    --   11.64  57.00 150.00   40
  7  \w     45.00  73.00   1.00  180.00    --   11.64  57.00 150.00   28
  8  \w     19.00  61.00   1.00  180.00    --  -13.67  18.00-141.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0190869000
_diffrn_orient_matrix_UB_12      -0.1274960000
_diffrn_orient_matrix_UB_13      -0.0462446000
_diffrn_orient_matrix_UB_21      -0.0182900000
_diffrn_orient_matrix_UB_22      0.0248263000
_diffrn_orient_matrix_UB_23      -0.2697006000
_diffrn_orient_matrix_UB_31      0.1239622000
_diffrn_orient_matrix_UB_32      -0.0158664000
_diffrn_orient_matrix_UB_33      -0.0469563000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            753
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.694
_diffrn_reflns_theta_min         5.238
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.882
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.248
_exptl_crystal_description       irregular
_exptl_crystal_F_000             73
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.590
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1438P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.2027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                129
_reflns_number_total             162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Moolooite_OP.cif
_cod_data_source_block           moolooite
_cod_original_cell_volume        77.50(5)
_cod_database_code               1569046
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cu1(0.125) C1(0.25)
;
_shelx_res_checksum              95938
_shelx_hkl_checksum              28168
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.596
_oxdiff_exptl_absorpt_empirical_full_min 0.459