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_1569047
_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             2022-11-29
_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                   5.607(2)
_cell_length_b                   5.428(2)
_cell_length_c                   2.5579(7)
_cell_measurement_reflns_used    382
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.6440
_cell_measurement_theta_min      5.2120
_cell_volume                     77.85(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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  (Sheldrick, 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.949
_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      0.0190489000
_diffrn_orient_matrix_UB_12      -0.1270739000
_diffrn_orient_matrix_UB_13      0.0490653000
_diffrn_orient_matrix_UB_21      0.0177066000
_diffrn_orient_matrix_UB_22      0.0259315000
_diffrn_orient_matrix_UB_23      0.2689122000
_diffrn_orient_matrix_UB_31      -0.1239242000
_diffrn_orient_matrix_UB_32      -0.0156712000
_diffrn_orient_matrix_UB_33      0.0458536000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       8
_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            382
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.947
_diffrn_reflns_theta_min         5.228
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    3.233
_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         1.836
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0810
_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^)+(0.1316P)^2^+0.3862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                316
_reflns_number_total             382
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 91.6237\% 
around [0.00 -0.00 1.00] (reciprocal) or [0.00 -0.00 1.00] (direct)
;
_cod_data_source_file            Moolooite_OP_twinned.cif
_cod_data_source_block           moolooite_twin1_hklf4
_cod_database_code               1569047
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Cu1 C2 O4'
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.662(13)
 0.338(13)
2. Others
 Fixed Sof: Cu1(0.125) C1(0.25)
;
_shelx_res_checksum              57554
_shelx_hkl_checksum              41547
_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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.632
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2