Synthesis of anionic alkaline earth metal methanesulfonates bearing photo-responsive methylviologen.
Chauhan, Aishwarya; Chauhan, Priyanka; Shankar, Ravi; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17014–17020; doi:10.1039/d4dt02229g

data_7717072
_publ_section_title
;
 Synthesis of anionic alkaline earth metal methanesulfonates bearing
 photo-responsive methylviologen.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17014
_journal_page_last               17020
_journal_paper_doi               10.1039/d4dt02229g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C6 H26 Ca2 O22 S6, C12 H14 N2'
_chemical_formula_sum            'C18 H40 Ca2 N2 O22 S6'
_chemical_formula_weight         909.071
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_block_doi                 10.5517/ccdc.csd.cc2k9q4r
_audit_creation_date             2024-07-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-08-05 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                88.105(4)
_cell_angle_beta                 84.771(4)
_cell_angle_gamma                79.178(4)
_cell_formula_units_Z            1
_cell_length_a                   5.8064(6)
_cell_length_b                   9.5980(11)
_cell_length_c                   16.929(2)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.16
_cell_volume                     922.69(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9985
_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_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.9994
_diffrn_reflns_Laue_measured_fraction_max 0.9985
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33514
_diffrn_reflns_point_group_measured_fraction_full 0.9994
_diffrn_reflns_point_group_measured_fraction_max 0.9985
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.16
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7100
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0613 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.9521.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             475.549
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.4023
_refine_diff_density_min         -0.6059
_refine_diff_density_rms         0.1476
_refine_ls_d_res_high            0.7482
_refine_ls_d_res_low             9.4260
_refine_ls_goodness_of_fit_ref   1.0291
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0291
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+0.2521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                4157
_reflns_number_total             4602
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02229g2.cif
_cod_data_source_block           2_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7717069--7717072.cif.'
_cod_original_cell_volume        922.67(18)
_cod_database_code               7717072
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H), C5(Ha), C4(Hb), C7(Hc)
2.b Idealised Me refined as rotating group:
 C9(Hd,He,Hf), C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C3(H3a,H3b,H3c)
;
_olex2_submission_special_instructions 'No special instructions were received'