Microwave−assisted synthesis: from a mononuclear {CoII} complex to {CoII9} solvomorphs
Collet, Alexandra; Wilson, Claire; Murrie, Mark; Dalton Transactions  (2018) –; doi:10.1039/C8DT04557G

data_7048359
_publ_section_title
;
 Microwave&#x2212;assisted synthesis: from a mononuclear {CoII} complex to
 {CoII9} solvomorphs
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT04557G
_journal_year                    2018
_chemical_formula_moiety         'C36 H64 Cl4 Co9 N6 O24, 12(H2O)'
_chemical_formula_sum            'C36 H88 Cl4 Co9 N6 O36'
_chemical_formula_weight         1853.29
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-11-12 deposited with the CCDC.
2018-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   39.2116(8)
_cell_length_b                   39.2116(8)
_cell_length_c                   11.7240(3)
_cell_measurement_reflns_used    9345
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.8230
_cell_measurement_theta_min      2.1540
_cell_volume                     15611.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -102.00  22.00   1.00   40.00    --  -13.10 -72.00 150.00  124
  2  \w    -42.00  76.00   1.00   40.00    --  -13.10  38.00  60.00  118
  3  \w    -48.00  -9.00   1.00   40.00    --  -13.10  72.00-150.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0057714000
_diffrn_orient_matrix_UB_12      -0.0117272000
_diffrn_orient_matrix_UB_13      0.0314900000
_diffrn_orient_matrix_UB_21      -0.0192008000
_diffrn_orient_matrix_UB_22      -0.0107812000
_diffrn_orient_matrix_UB_23      0.0233879000
_diffrn_orient_matrix_UB_31      -0.0058166000
_diffrn_orient_matrix_UB_32      -0.0135229000
_diffrn_orient_matrix_UB_33      -0.0460541000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            38042
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.353
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_description       needle
_exptl_crystal_F_000             8505
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.105
_refine_diff_density_min         -1.633
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         7930
_refine_ls_number_restraints     483
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+115.5571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6410
_reflns_number_total             7930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04557g2.cif
_cod_data_source_block           complex2plus12H2O
_cod_original_cell_volume        15611.2(8)
_cod_database_code               7048359
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     'AC663blue (needle)'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 O6-H6
 0.85 with sigma of 0.01
 C2-H1
 1.921235 with sigma of 0.02
 Co2-H1
 2.817887 with sigma of 0.02
 C10-H6
 1.904863 with sigma of 0.02
 Co3-H6
 2.779812 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C18(H18A,H18B), C7(H7A,H7B), C11(H11A,H11B), C14(H14A,H14B),
 C1(H1A,H1B), C3(H3A,H3B), C15(H15A,H15B), C8(H8A,H8B), C4(H4A,H4B), C17(H17A,
 H17B), C2(H2A,H2B), C5(H5A,H5B), C9(H9A,H9B), C10(H10A,H10B)
;
_shelx_res_checksum              61464
_shelx_fab_checksum              63331
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.603
_oxdiff_exptl_absorpt_empirical_full_min 0.656