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_7717071
_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         'C12 H44 Ca4 O40 S12, 2(C8 H20 N2)'
_chemical_formula_sum            'C28 H84 Ca4 N4 O40 S12'
_chemical_formula_weight         1662.088
_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_Int_Tables_number      14
_audit_block_doi                 10.5517/ccdc.csd.cc2k9q5s
_audit_creation_date             2023-04-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-06-14 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 93.49(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            1
_cell_length_a                   5.805(2)
_cell_length_b                   31.377(6)
_cell_length_c                   9.185(2)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.264
_cell_measurement_theta_min      2.314
_cell_volume                     1669.9(8)
_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      296.00
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.9993
_diffrn_reflns_Laue_measured_fraction_max 0.9995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            38575
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9995
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.31
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6965
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0997 before and 0.0713 after correction.
The Ratio of minimum to maximum transmission is 0.9340.
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    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             875.024
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.7105
_refine_diff_density_min         -0.7764
_refine_diff_density_rms         0.1914
_refine_ls_d_res_high            0.7502
_refine_ls_d_res_low             8.8005
_refine_ls_goodness_of_fit_ref   0.9853
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9853
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+0.4329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              41
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                3775
_reflns_number_total             4132
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02229g2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7717069--7717072.cif.'
_cod_database_code               7717071
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1c,H1d), C2(H2a,H2b)
2.b Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C6(H6a,H6b,H6c), C5(H5a,
 H5b,H5c)
;
_olex2_submission_special_instructions 'No special instructions were received'