Designing Cr complexes for a neutral Fe-Cr redox flow battery.
Ruan, Wenqing; Mao, Jiatao; Yang, Shida; Shi, Chuan; Jia, Guochen; Chen, Qing; Chemical communications (Cambridge, England) 56 (2020) 3171–3174; doi:10.1039/c9cc09704j

data_7125979
_publ_section_title
;
 Designing Cr complexes for a neutral Fe-Cr redox flow battery.
;
_journal_issue                   21
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3171
_journal_page_last               3174
_journal_paper_doi               10.1039/c9cc09704j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'Br, C26 H34 Cr N4 O10, 3.75(H2 O), 0.5(C3 H6 O)'
_chemical_formula_sum            'C27.5 H44.5 Br Cr N4 O14.25'
_chemical_formula_weight         791.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-11-28 deposited with the CCDC.	2020-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                75.374(7)
_cell_angle_beta                 79.253(7)
_cell_angle_gamma                72.060(7)
_cell_formula_units_Z            2
_cell_length_a                   9.8426(7)
_cell_length_b                   12.5393(9)
_cell_length_c                   16.1571(15)
_cell_measurement_reflns_used    4750
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.1000
_cell_measurement_theta_min      3.7660
_cell_volume                     1822.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.973
_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     28.00 141.00   1.00   15.00    --  106.99 -77.00  90.00  113
  2  \w   -115.00 -14.00   1.00    5.00    --  -40.32 -37.00 150.00  101
  3  \w   -115.00 -73.00   1.00    5.00    --  -40.32-145.00-106.00   42
  4  \w   -113.00 -14.00   1.00    5.00    --  -40.32 -37.00-120.00   99
  5  \w      2.00  82.00   1.00    5.00    --   40.32 -99.00 120.00   80
  6  \w     42.00 138.00   1.00   15.00    --  106.99 -30.00 150.00   96
  7  \w     79.00 170.00   1.00   15.00    --  106.99  45.00-180.00   91
  8  \w     48.00 116.00   1.00   15.00    --  106.99-125.00  90.00   68
  9  \w     32.00 109.00   1.00   15.00    --  106.99 -45.00 -90.00   77
 10  \w     33.00 109.00   1.00   15.00    --  106.99 -94.00 -90.00   76
 11  \w     24.00 163.00   1.00   15.00    --  106.99 -15.00   0.00  139
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1647227000
_diffrn_orient_matrix_UB_12      -0.0447006000
_diffrn_orient_matrix_UB_13      -0.0178380000
_diffrn_orient_matrix_UB_21      0.0092170000
_diffrn_orient_matrix_UB_22      -0.0440405000
_diffrn_orient_matrix_UB_23      0.0974020000
_diffrn_orient_matrix_UB_31      -0.0151860000
_diffrn_orient_matrix_UB_32      -0.1161814000
_diffrn_orient_matrix_UB_33      -0.0065210000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10051
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.499
_diffrn_reflns_theta_min         3.789
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.457
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       plate
_exptl_crystal_F_000             821
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6390
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0980P)^2^+1.8500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5577
_reflns_number_total             6390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09704j2.cif
_cod_data_source_block           ruan53d
_cod_depositor_comments          'Adding full bibliography for 7125979.cif.'
_cod_original_formula_sum        'C27.50 H44.50 Br Cr N4 O14.25'
_cod_database_code               7125979
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.469
_reflns_odcompleteness_completeness 98.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C1S-C3S \\sim C1S-C2S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.003
4. Others
 Fixed Sof: Br1(0.17) Br1A(0.66) Br1B(0.17) O1S(0.5) C1S(0.5) C2S(0.5)
 H2SA(0.5) H2SB(0.5) H2SC(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) H3SC(0.5) O4W(0.75)
 H4WA(0.75) H4WB(0.75)
5.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C23(H23), C25(H25)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C2S(H2SA,H2SB,H2SC), C3S(H3SA,
 H3SB,H3SC)
;
_shelx_res_checksum              59400
_olex2_date_sample_data_collection 2019-04-12
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.445
_oxdiff_exptl_absorpt_empirical_full_min 0.789