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_1551371
_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         '2(Mn O42 W17 Na1 F6), O44, Cs11, K5'
_chemical_formula_sum            'Cs11 F12 K5 Mn2 Na2 O128 W34'
_chemical_formula_weight         10340.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.983(4)
_cell_length_b                   18.413(4)
_cell_length_c                   22.333(5)
_cell_measurement_reflns_used    19035
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.2
_cell_volume                     7395(3)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker KappaApexII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19035
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         2.868
_exptl_absorpt_coefficient_mu    29.412
_exptl_absorpt_correction_T_max  0.410
_exptl_absorpt_correction_T_min  0.105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Apex2'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.644
_exptl_crystal_description       plate
_exptl_crystal_F_000             8840
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         4.738
_refine_diff_density_min         -3.147
_refine_diff_density_rms         0.471
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         3499
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0787
_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^)+(0.0500P)^2^+2105.6692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2001
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2833
_reflns_number_total             3499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2675-s3.cif
_cod_data_source_block           n678
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_sg_symbol_H-M      'C m c a'
_cod_database_code               1551371
_shelx_estimated_absorpt_t_min   0.126
_shelx_estimated_absorpt_t_max   0.386
_shelx_res_checksum              72040
_shelx_hkl_checksum              41532