Real-time molecular scale observation of crystal formation
Roy E. Schreiber; Lothar Houben; Sharon G. Wolf; Gregory Leitus; Zhong-Ling Lang; Jorge J. Carbo; Josep M. Poblet; Ronny Neumann; Nature Chemistry 9 (2017) 369–373; doi:10.1038/nchem.2675

data_1551370
_publ_section_title
;
 Real-time molecular scale observation of crystal formation
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              369
_journal_page_last               373
_journal_paper_doi               10.1038/nchem.2675
_journal_volume                  9
_journal_year                    2017
_chemical_formula_moiety         'Na F6 Mn O56 W17, 6(K), 2(Na) , 20(O)'
_chemical_formula_sum            'F6 K6 Mn Na3 O76 W17'
_chemical_formula_weight         4813.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 92.34(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.586(5)
_cell_length_b                   12.292(3)
_cell_length_c                   29.421(6)
_cell_measurement_reflns_used    19886
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     8161(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELEXT
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.0945
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            19886
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         3.246
_exptl_absorpt_coefficient_mu    24.439
_exptl_absorpt_correction_T_max  0.367
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Nonius Kappa CCD'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.918
_exptl_crystal_description       plate
_exptl_crystal_F_000             8368
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.707
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.424
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7399
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0534P)^2^+24.2448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5067
_reflns_number_total             7399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2675-s2.cif
_cod_data_source_block           n581
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1551370
_shelx_estimated_absorpt_t_min   0.096
_shelx_estimated_absorpt_t_max   0.375
_shelx_res_checksum              59039
_shelx_hkl_checksum              16121