Crystal structure of the high-P polymorph of Ca2B6O6(OH)10·2(H2O) (meyerhofferite)
Comboni, Davide; Poreba, Tomasz; Pagliaro, Francesco; Battiston, Tommaso; Lotti, Paolo; Gatta, Giacomo Diego; Garbarino, Gaston; Hanfland, Michael; Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials 77 (2021) 940–945; doi:10.1107/S2052520621009768

data_2022903
_publ_section_title
;
 Crystal structure of the high-P polymorph of Ca2B6O6(OH)10&#x00B7;2(H2O)
 (meyerhofferite)
;
_journal_coeditor_code           DK5106
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials'
_journal_page_first              940
_journal_page_last               945
_journal_paper_doi               10.1107/S2052520621009768
_journal_volume                  77
_journal_year                    2021
_chemical_formula_structural     'Ca (B3 O3 (O H)5) (H2 O)'
_chemical_formula_sum            'B3 Ca H7 O9'
_chemical_formula_weight         223.6
_chemical_name_common            meyerhofferite
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2021-04-028
_audit_creation_method
;
'Jana2006 Version : 14/01/2019'
;
_cell_angle_alpha                89.922(3)
_cell_angle_beta                 103.380(10)
_cell_angle_gamma                86.859(10)
_cell_formula_units_Z            2
_cell_length_a                   6.465(3)
_cell_length_b                   8.059(3)
_cell_length_c                   6.388(3)
_cell_measurement_pressure       3140000
_cell_measurement_reflns_used    718
_cell_measurement_temperature    293
_cell_measurement_theta_max      19.5850
_cell_measurement_theta_min      2.3780
_cell_volume                     323.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'Jana2006 (Petricek et al., 2014)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_diffrn_ambient_pressure         3140000
_diffrn_ambient_temperature      293(1)
_diffrn_detector                 'Eiger2 9M CdTe'
_diffrn_measured_fraction_theta_full 0.30
_diffrn_measured_fraction_theta_max 0.16
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
RUN    TYPE OF SCAN  START(DEG)   END(DEG)    # FRAMES    EXP(SEC)   OMEGA(DEG)  THETA(DEG)  KAPPA(DEG)   PHI(DEG) 
Run 1 Omega scan: (-32.000 - 32.000,128 frames, 0.200 sec, 0.500 deg) at th=0.000, ka=0.000,ph=0.000 (rot geo dd=199.206)
  1       OMEGA       -32.00000    32.00000         128      0.20000    n/a        -0.01874     0.00000     0.00000
;
_diffrn_measurement_device       ID15b
_diffrn_measurement_device_type  beamline
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.065312
_diffrn_orient_matrix_UB_12      0.005584
_diffrn_orient_matrix_UB_13      -0.013494
_diffrn_orient_matrix_UB_21      0.003872
_diffrn_orient_matrix_UB_22      0.047299
_diffrn_orient_matrix_UB_23      0.023853
_diffrn_orient_matrix_UB_31      -0.000466
_diffrn_orient_matrix_UB_32      0.018331
_diffrn_orient_matrix_UB_33      -0.060132
_diffrn_radiation_collimation    '0.2 mm  double pinhole'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41066
_diffrn_reflns_av_R_equivalents  0.0126
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            718
_diffrn_reflns_theta_full        12.09
_diffrn_reflns_theta_max         19.59
_diffrn_reflns_theta_min         2.28
_diffrn_source                   'ESRF: Synchrotron radiation'
_diffrn_source_power             '200 mA'
_diffrn_source_type              'undulator, IVU20c'
_diffrn_source_voltage           30keV
_diffrn_standards_decay_%        0.5(1)
_diffrn_standards_interval_count 15
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.2244
_exptl_crystal_description       'prismatic habit'
_exptl_crystal_F_000             214
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.27
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    3.63
_refine_ls_goodness_of_fit_ref   3.48
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_constraints    0
_refine_ls_number_parameters     53
_refine_ls_number_reflns         479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.0148
_refine_ls_shift/su_mean         0.0041
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0627
_reflns_number_gt                437
_reflns_number_total             479
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            dk5106sup1.cif
_cod_data_source_block           I_3.14GPa
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_formula_sum        'H7 B3 Ca1 O9'
_cod_database_code               2022903
_cod_database_fobs_code 2022903