Crystal structure determination of a lifelong biopersistent asbestos fibre using single-crystal synchrotron X-ray micro-diffraction
Giacobbe, Carlotta; Di Giuseppe, Dario; Zoboli, Alessandro; Lassinantti Gualtieri, Magdalena; Bonasoni, Paola; Moliterni, Anna; Corriero, Nicola; Altomare, Angela; Wright, Jonathan; Gualtieri, Alessandro F.; IUCrJ 8 (2021) 76–86; doi:10.1107/S2052252520015079

data_1559801
_publ_section_title
;
 Crystal structure determination of a lifelong biopersistent asbestos
 fibre using single-crystal synchrotron X-ray micro-diffraction
;
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_page_first              76
_journal_page_last               86
_journal_paper_doi               10.1107/S2052252520015079
_journal_volume                  8
_journal_year                    2021
_chemical_formula_sum
'Al0.17 Ca0.18 F0.08 Fe5.4 H1.92 Mg1.25 O23.92 Si8'
_chemical_formula_weight         954.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-03-28 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 101.883(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.54396(20)
_cell_length_b                   18.2455(4)
_cell_length_c                   5.32660(12)
_cell_measurement_reflns_used    1070
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.78
_cell_measurement_theta_min      1.72
_cell_volume                     907.67(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'ID11 diffractometer'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.30909
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7498
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        10.688
_diffrn_reflns_theta_max         11.886
_diffrn_reflns_theta_min         1.699
_diffrn_source                   synchrotron
_diffrn_standards_interval_time  0.0
_diffrn_standards_number         1089
_exptl_absorpt_coefficient_mu    0.5
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK; Oxford Diffraction, (2006)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    3.493
_exptl_crystal_description       needle
_exptl_crystal_F_000             934.5
_exptl_crystal_size_max          0.001
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_exptl_transmission_factor_max   0.97
_exptl_transmission_factor_min   0.91
_refine_diff_density_max         1.275
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1089
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0581P)^2^+17.3651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                986
_reflns_number_total             1089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ro5022.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 1559801--1559803.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum
'Ca0.18 Fe5.40 Al0.17 Mg1.25 Si8 O23.92 F0.08 H1.92'
_cod_database_code               1559801
_publcif_datablock.id            {f36309ef-3c22-480d-ba1a-fb7336d765c7}
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   1.000
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              87428
_shelx_hkl_checksum              72026
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n