Network diversity through two-step crystal engineering of a decorated 6-connected primary molecular building block
Yang, Qing-Yuan; Chen, Kai-Jie; Schoedel, Alexander; Wojtas, Lukasz; Perry IV, John J.; Zaworotko, Michael J.; CrystEngComm 18 (2016) 8578–; doi:10.1039/C6CE01544A

data_7236183
_publ_section_title
;
 Network diversity through two-step crystal engineering of a decorated
 6-connected primary molecular building block
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              8578
_journal_paper_doi               10.1039/C6CE01544A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.5(C156 H96 Cl12 Cr12 Mn6 N24 O64), 6(O)'
_chemical_formula_sum            'C78 H84 Cl6 Cr6 Mn3 N14 O44'
_chemical_formula_weight         2611.11
_space_group_crystal_system      hexagonal
_space_group_IT_number           193
_space_group_name_Hall           '-P 6c 2'
_space_group_name_H-M_alt        'P 63/m c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_audit_update_record
;
2016-09-30 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   22.045(2)
_cell_length_b                   22.045(2)
_cell_length_c                   21.768(2)
_cell_measurement_reflns_used    1978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.1
_cell_measurement_theta_min      1.2
_cell_volume                     9161.6(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31739
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        14.096
_diffrn_reflns_theta_max         14.096
_diffrn_reflns_theta_min         1.204
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.9974
_exptl_absorpt_correction_T_min  0.9935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.947
_exptl_crystal_description       needle
_exptl_crystal_F_000             2646
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2824
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0601
_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^)+(0.1311P)^2^+12.3736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1835
_reflns_number_total             2824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01544a2.cif
_cod_data_source_block           PMBB-2-stp-1
_cod_original_cell_volume        9161.6(19)
_cod_database_code               7236183
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O21-C22 = O21-C21
 1.4 with sigma of 0.02
3. Others
 Fixed Sof: C21(0.25) C22(0.25) O22(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15)
;
_shelx_fab_checksum              52814
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'