Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination
Krause, Lennard; Herbst-Irmer, Regine; Sheldrick, George M.; Stalke, Dietmar; Journal of Applied Crystallography 48 (2015) –; doi:10.1107/S1600576714022985

data_2300495
_publ_section_title
;
 Comparison of silver and molybdenum microfocus X-ray sources for
 single-crystal structure determination
;
_journal_coeditor_code           aj5242
_journal_issue                   1
_journal_name_full               'Journal of Applied Crystallography'
_journal_paper_doi               10.1107/S1600576714022985
_journal_volume                  48
_journal_year                    2015
_chemical_formula_moiety         'C30 H46 Br2 Cl2 Co N4 Si2'
_chemical_formula_sum            'C30 H46 Br2 Cl2 Co N4 Si2'
_chemical_formula_weight         808.54
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 102.95(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.568(3)
_cell_length_b                   9.504(2)
_cell_length_c                   21.378(3)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.7875
_cell_measurement_theta_min      2.603
_cell_volume                     3676.6(11)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            60559
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.820
_diffrn_reflns_theta_min         1.543
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  0.9597
_exptl_absorpt_correction_T_min  0.8407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         7811
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+1.9900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6882
_reflns_number_total             7811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aj5242sup1.cif
_cod_data_source_block           6-(Ag)
_cod_database_code               2300495
_cod_database_fobs_code          2300495
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.970
_shelxl_version_number           2014-3
_shelx_res_checksum              97442
_shelx_hkl_checksum              70109