A versatile environmental control cell for <i>in situ</i> guest exchange single-crystal diffraction
Cox, Jordan M.; Walton, Ian M.; Benson, Cassidy A.; Chen, Yu-Sheng; Benedict, Jason B.; Journal of Applied Crystallography 48 (2015) 578–581; doi:10.1107/S160057671500432X

data_2300502
_publ_section_title
;
 A versatile environmental control cell for <i>in situ</i> guest exchange
 single-crystal diffraction
;
_journal_coeditor_code           KC5005SUP1
_journal_issue                   2
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              578
_journal_page_last               581
_journal_paper_doi               10.1107/S160057671500432X
_journal_volume                  48
_journal_year                    2015
_chemical_formula_moiety         'C13 H11 Co N2 O5, 2(H2 O)'
_chemical_formula_sum            'C13 H15 Co N2 O7'
_chemical_formula_weight         370.20
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-23 # Formatted by IUCr publCIF system
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.5410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6105(6)
_cell_length_b                   7.6858(3)
_cell_length_c                   15.9256(7)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.17
_cell_measurement_theta_min      2.62
_cell_volume                     1479.66(11)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28364
_diffrn_reflns_theta_full        17.18
_diffrn_reflns_theta_max         17.18
_diffrn_reflns_theta_min         1.55
_diffrn_source                   synchrotron
_diffrn_source_type              'Bending magnet, ID-15B, APS, ANL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.7137
_exptl_absorpt_correction_T_min  0.6170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1579 before and 0.1047 after correction.
The Ratio of minimum to maximum transmission is 0.8645.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.610
_refine_diff_density_min         -1.729
_refine_diff_density_rms         0.328
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         4261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0872
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1592P)^2^+0.5543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2223
_refine_ls_wR_factor_ref         0.2344
_reflns_number_gt                3722
_reflns_number_total             4261
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            kc5005sup1.cf
_cod_data_source_block           I
_cod_database_code               2300502
_publcif_datablock.id            {1861bdb4-d9d6-4d71-9cfd-06256c4101dc}
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O7(H7A,H7B), O6(H6A,H6B)
2.b Rotating group:
 O5(H5A,H5B)
2.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C5(H5), C13(H13), C9(H9), C12(H12), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n